3-Sep-21 News Discovery of 40545-33-3

The synthetic route of 40545-33-3 has been constantly updated, and we look forward to future research findings.

Related Products of 40545-33-3, A common heterocyclic compound, 40545-33-3, name is 2-Amino-5-methylbenzamide, molecular formula is C8H10N2O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of 2-amino-5-methylbenzamide (150 mg, 1 mmol)), Benzaldehyde (106 mg, lmmol), Water (1 · OmL)And then added to 5mL single-mouth bottle. The mixture was reacted at reflux temperature for 2 hours and then cooled to room temperature. Then join[Cp * Ir (H20) 3] [0Tf] 2 (6.8 mg, 0. ol mmol, 1 mol%) was reacted at reflux temperature for 1 hour and then cooled to room temperatureTheThe solvent was removed under vacuum under reduced pressure and then passed through a column chromatography (developing solvent): Ethyl acetate / n-hexane) to give the pure title compoundObjects,Yield: 81%.

The synthetic route of 40545-33-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing University of Science and Technology; LI, Feng; LU, Lei; MA, Juan; CHENG, Rui; (18 pag.)CN106518789; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3-Sep-21 News Introduction of a new synthetic route about 6331-71-1

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 6331-71-1, name is 4-Amino-N,N-dimethylbenzamide, A new synthetic method of this compound is introduced below., Formula: C9H12N2O

To a mixture of B-02b (1.68 g, 10.2 mmol) in 30 mL concentrated hydrochloric acid at -10 0C is added a solution of sodium nitrite (755 mg, 10.9 mmol) in 7 mL water. The reaction mixture is stirred for 1 h at 0 0C and then at -5 0C a solution of tin(II) chloride dehydrate (4.81 g, 21.4 mmol) in 10 mL concentrated HCl is added. The cooling bath is removed and the reaction mixture is stirred for 1 h at RT. The reaction mixture is basified with 8 M aqueous sodium hydroxide and extracted with ethyl acetate. The combined organic phases are dried over MgSO4 and concentrated in vacuo. The residue is taken up in diethyl ether and 2 M HCl in diethyl ether is added until no more precipitate is formed. The precipitate is filtered of and dried in vacuo at 40 0C. Yield: 213 mg.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WO2009/112565; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3-Sep-21 News Continuously updated synthesis method about 4141-08-6

The synthetic route of 4141-08-6 has been constantly updated, and we look forward to future research findings.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4141-08-6, name is 2-Amino-N-methylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: amides-buliding-blocks

2-amino-N-methylbenzamide (1.53 g, 10 mmol), potassium carbonate (2.07 g, 15 mmol), DMF (15 mL) were added in a 100 mL reaction flask, 2,4,5-trichloropyrimidine (1.85 g, 10 mmol) was added with stirring. The reaction solution was stirred at 75 C for 5 hours, the reaction solution was poured into water, and the solid precipitated, and the filter cake was collected by filtration. The filter cake was beaten with 50% acetonitrile-water and dried to give 2 g of pale yellow solid II-01 in 67% yield.

The synthetic route of 4141-08-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Normal University; Zhang Huabei; Fang Yu; Wang Dawei; Qi Yueheng; Liu Jianping; Gao Hang; (43 pag.)CN106905303; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3-Sep-2021 News Analyzing the synthesis route of 63920-73-0

According to the analysis of related databases, 63920-73-0, the application of this compound in the production field has become more and more popular.

Related Products of 63920-73-0, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 63920-73-0 as follows.

A mixture of 2-amino-4,6-dimethoxy-benzamide (0.71 g, 3.71 mmol), 3,5-dimethyl-4-benzyloxy benzaldehyde (0.94 g, 3.90 mmol), sodium hydrogensulfite (0.68 g, 3.90 mmol) and p-toluenesulfonic acid (70 mg, 0.37 mmol) in N,N-dimethylacetamide (25 mL) was stirred at 150 C. for 16 h. The reaction mixture was cooled to room temperature and diluted with water (200 mL). The resulting solid was collected by filtration and washed with hexanes to afford 2-(4-benzyloxy-3,5-dimethyl-phenyl)-5,7-dimethoxy-3H-quinazolin-4-one as a white solid (1.2 g, 79%).

According to the analysis of related databases, 63920-73-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RVX Therapeutics Inc.; McLure, Kevin G.; Young, Peter Ronald; US2013/281397; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3-Sep-2021 News Some tips on 7341-96-0

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Propiolamide, other downstream synthetic routes, hurry up and to see.

Electric Literature of 7341-96-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 7341-96-0, name is Propiolamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and phenyl diazonium acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is shown as formula (f) is shown. The yield is 89%, dr value is equal to the 88:12. The product of the1As shown in Figure 11, H NMR schematic view thereof13C NMR schematic view as shown in Figure 12.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Propiolamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3-Sep-2021 News Extended knowledge of 4141-08-6

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 4141-08-6.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 4141-08-6, name is 2-Amino-N-methylbenzamide, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Amino-N-methylbenzamide

In a 250 mL reaction flask,A solution of 15 g (0.1 mol) of 2-amino-N-methylbenzamide,80 mL of acetonitrile was added,Ice bath temperature control below 10 ,33.75 g (0.25 mol) of sulfonyl chloride was slowly added dropwise,30min drops finished,Stirred at room temperature for 3 h,Most of the acetonitrile was distilled off under reduced pressure,With 20% Na2CO3 aqueous solution to adjust the pH to neutral,Filter,Washed,19.8 g of an off-white solid,Yield 90.4%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 4141-08-6.

Reference:
Patent; Qingdao University of Science and Technology; XU, LIANGZHONG; TIAN, SHUAIWANG; WANG, MINGHUI; (9 pag.)CN105153113; (2016); B;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

September 2,2021 News Brief introduction of 104060-23-3

The synthetic route of N-Boc-2-(4-Aminophenyl)ethanol has been constantly updated, and we look forward to future research findings.

Reference of 104060-23-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 104060-23-3, name is N-Boc-2-(4-Aminophenyl)ethanol belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 4: Preparation of compounds according to the invention.Diphenylphosphonylated compounds according to the invention (as e.g. in example 2) were prepared according to Scheme 1 , by a fast and convenient synthetic route, affording the opportunity to obtain large and diverse series of compounds. The aminophosphonate building block was prepared from fe/t-butylcarbamate protected 4- aminophenylacetaldehyde (12), prepared from the corresponding alcohol (11) with Dess- Martin periodinane (Dess, D. B. and Martin, J. C. Readily Accessible 12-1-5 Oxidant for the Conversion of Primary and Secondary Alcohols to Aldehydes and Ketones. J. Org. Chem., 1983, 48, 4155-4156.). An amidoalkylation reaction with benzylcarbamate and triphenylphosphite using copper triflate as catalyst, afforded lambda/-benzyloxycarbonyl protected diphenyl phosphonate 13 (Van der Veken, P.; El Sayed, I.; Joossens, J.; Stevens, C. V.; Augustyns, K. and Haemers, A.; Lewis Acid Catalyzed Synthesis of N- Protected Diphenyl 1-Aminoalkyl-Phosphonates. Synthesis, 2005, 4, 634-638). Acidolysis removed the terf-butyl carbamate protecting group. lambda/,lambda/’-bis(te/-butoxycarbonyl)-1- guanylpyrazole was used to introduce the protected guanidine group (Drake, B.; Patek, M.; Lebl, M., A Convenient Preparation of Monosubstituted N,N’-Di(Boc)-Protected Guanidines. Synthesis, 1994, 579-582.). Compound 14 was subsequently deprotected under hydrogenolytic conditions. Small non-peptide guanidyl compounds (7) were made by coupling compound (15) with selected sulfonyl chlorides or acylchlorides in pyridine. EPO The p-acetylaminophenyl phosphonates (as e.g. in example 3) were prepared following scheme 1 using tri-p-acetylaminophenylphosphite (Belyaev et al. A. Structure-Activity Relationship of Diaryl Phosphonate Esters as Potent Irreversible Dipeptidyl Peptidase IV Inhibitors. J.Med. Chem., 1999, 42, 1041-1052) (22).4-(tert-Butyloxycarbonylamino)phenylacetaldehyde (intermediate No. 12 in scheme1 ).Yield: 58%1H NMR (CDCI3, 400MHz) delta 1.5 (s, 9H)1 3.75 (d, 2H), 7.10 (d, 2H), 7.30 (m, 2H), 9.6 (t, 1 H)MS (ESI): m/z (M+Na)258, (M+Me0H+Na) 290Dess-Martin Oxidation: To a stirred suspension of alcohol (1 eq.) in DCM (80ml) at -78 0C, a solution of Dess-Martin periodane (1.5 eq from a 15wt% solution) was added. The suspension was stirred for 3h at room temperature. The resulting solution was poured into a vigorously stirred saturated NaHCO3 and Na2S2O3 solution (1 :1 100ml). The organic layer was separated and washed with brine and dried over Na2SO4. The crude product was obtained by removing the solvent in vacuo.tert-Butyl 4-(2-oxoethyl)phenylcarbamate (12)2-(4-Aminophenyl)ethanol (13.7 g, 0.1 mol) was dissolved in dioxane (120 ml). Triethylamine (10.1 g, 0.1 mol) was added followed by addition of Boc2O (21.8 g, 0.1 mol). The reaction mixture was stirred overnight. After evaporation under vacuum, the residue EPO was dissolved in ethylacetate and washed with HCI (2N) and brine. The organic layer was dried over Na2SO4 and evaporated. Purification by flash chromatography afforded the tert- butyl 4-(2-hydroxyethyl)phenylcarbamate as a white solid (19 g, 80 mmol, 80%). To a stirred solution of this alcohol (1eq) in dichloromethane, a solution of Dess-Martin periodane (1.2 eq from 15% wt solution) was added. The suspension was stirred for 4 h at room temperature. The resulting solution was poured into a vigorously stirred saturated solution of NaHCO3 and Na2S2O3 (1 : 1, 100 ml). The organic layer was separated and washed with brine and dried over anhydrous Na2SO4. This crude aldehyde 12 was used directly for further reaction.

The synthetic route of N-Boc-2-(4-Aminophenyl)ethanol has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITEIT ANTWERPEN; WO2007/45496; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

9/2/21 News Brief introduction of 201162-53-0

The synthetic route of 3-Boc-3,8-Diazabicyclo[3.2.1]octane has been constantly updated, and we look forward to future research findings.

Reference of 201162-53-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 201162-53-0, name is 3-Boc-3,8-Diazabicyclo[3.2.1]octane belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Into a 250-mL round-bottom flask, was placed a solution of 2-bromo-4-fluoropyridine (7.8 g, 44.32 mmol, 1.05 equiv), tert-butyl 3,8-diazabicyclo[3.2.1]octane-3-carboxylate (9 g, 42.4 mmol, 1.00 equiv), DIEA (25 g, 193 mmol, 4.00 equiv) in NMP (120 mL). The resulting solution was stirred for 3 hours at 150 C. The reaction mixture was cooled. The reaction was then quenched by the addition of water (200 mL). The resulting solution was extracted with ethyl acetate (50 mL*3), and the organic layers were combined. The resulting mixture was washed with water (50 mL*1) and brine (50 mL*1). The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column eluting with ethyl acetate/petroleum ether (1:2). This resulted in 11.7 g (75%) of tert-butyl 8-(2-bromopyridin-4-yl)-3,8-diazabicyclo[3.2.1]octane-3-carboxylate as a yellow solid.

The synthetic route of 3-Boc-3,8-Diazabicyclo[3.2.1]octane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Arvinas Operations, Inc.; Genentech, Inc.; Crew, Andrew P.; Wang, Jing; Berlin, Michael; Dragovich, Peter; Chen, Huifen; Staben, Leanna; US2019/300521; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

9/2/21 News Application of 406233-31-6

The synthetic route of 406233-31-6 has been constantly updated, and we look forward to future research findings.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 406233-31-6, name is 4-Fluoro-3-nitrobenzenesulfonamide, A new synthetic method of this compound is introduced below., Recommanded Product: 4-Fluoro-3-nitrobenzenesulfonamide

To a mixture of 4-fluoro-3-nitrobenzenesulfonamide (1 g, 4.54 mmol) and compound tert-butyl 4-fluoro-4- (hydroxymethyl) piperidine-1-carboxylate (1.06 g, 4.54 mmol) in THF (20 mL) was added NaH (726.61 mg, 18.17 mmol, 60%purity) in one portion at 0C under N 2. The mixture was stirred at 15C for 14 hours. TLC showed the reaction was completed. 20 mL saturated NH 4Cl solution was added to the mixture, the aqueous phase was extracted with ethyl acetate (20 mL x 3). The combined organic phase was washed with brine (50 mL), dried with anhydrous Na 2SO 4, filtered and concentrated in vacuum. The crude product was purified by re-crystallization in EtOAc (10 mL) to give tert-butyl 4-fluoro-4- ((2-nitro-4-sulfamoylphenoxy) methyl) piperidine-1-carboxylate (1.17 g, 2.70 mmol, 59.4% yield) as yellow solid. 1H NMR (400MHz, DMSO-d 6) delta ppm: 8.31 (br s, 1H), 8.06 (br d, J = 8.6 Hz, 1H), 7.64-7.54 (m, 1H), 7.25 (br s, 2H), 4.48-4.33 (m, 2H), 3.84 (br d, J = 11.9 Hz, 2H), 3.03 (br s, 2H), 1.97-1.84 (m, 2H), 1.82-1.61 (m, 2H), 1.41 (d, J = 2.9 Hz, 9H).

The synthetic route of 406233-31-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BEIGENE, LTD.; GUO, Yunhang; XUE, Hai; WANG, Zhiwei; SUN, Hanzi; (493 pag.)WO2019/210828; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

9/2/21 News Share a compound : 118753-70-1

The synthetic route of tert-Butyl bis(2-chloroethyl)carbamate has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 118753-70-1, name is tert-Butyl bis(2-chloroethyl)carbamate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Quality Control of tert-Butyl bis(2-chloroethyl)carbamate

Reference example 79; (1); To compound (1) (4.0g) in DMSO (60ml) was gradually added 60percent sodium hydride (1.35g) under ice-cooling, and the mixture was stirred at 0°C for 1 hour. Thereto was dropped N – tert-butoxycarbonyl-N,N-bis(2-chloroethyl)amine (4.59g) in DMSO (30ml) and the mixture was stirred at room temperature for 3 hours. The reaction mixture was poured to ice water, and the mixture was extracted with methylene chloride. The extract was washed with water, and dried. After removal of the solvent, the residue was purified with NH-silica gel chromatography (hexane/ethyl acetate=100/0–>100/20) to give compound (2) (2.03g) as a yellow oily product. APCI-MS (m/e): 265/267 (M+2H-BOC)+

The synthetic route of tert-Butyl bis(2-chloroethyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; EP1956009; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics