Month: August 2021

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 37394-93-7 as follows. Quality Control of 2-Chloro-N-(o-tolyl)acetamide

General procedure: A mixture of 5a-j (18 mmol) and KI (4.4 g, 27 mmol) inacetone (40 mL) was refluxed for 2 h, and the solvent was evaporated in vacuo. Water was added, and the solids were collected and dried to give compounds 6a-j.

According to the analysis of related databases, 37394-93-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhu, Xiong; Fu, Junjie; Tang, Yan; Gao, Yuan; Zhang, Shijin; Guo, Qinglong; Bioorganic and Medicinal Chemistry Letters; vol. 26; 4; (2016); p. 1360 – 1364;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 120157-97-3, 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. 120157-97-3, name is N-Boc-2-(4-Bromophenyl)ethylamine belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of teit-butyl N-[2-(4-bromophenyl)ethyl]carbamate, Intermediate 29 (4.09 g,13.6 mmol), [4-cyanomethyl)phenyl]boronic acid (2.63 g, 16.4 mmol) and K2C03 (5.65 g,40.9 mmol) in 1,4-dioxane (105 ml) was degassed by bubbling a stream nitrogen throughthe mixture for 5 mm. Pd(dppf)C12.CH2CI2 (445 mg, 0.545 mmol) was added anddegassing was continued for a further 5 mm. The reaction mixture was heated at 80 Cfor 15 h then at 100 C for 7 h. The reaction was allowed to cool to RT then retreated with K2C03 (3.76 g, 27.2 mmol) and degassed for 5 mm. Pd(dppf)C12.CH2CI2 (445 mg, 0.545 mmol) was added then the mixture was degassed for a further 5 mm. The resultant mixture was heated at 100 C for 24 h then allowed to cool to RT. The reaction wasretreated with K2C03 (1.88 g, 13.6 mmol) and [4-cyanomethyl)phenyl]boronic acid (0.88 g, 5.5 mmol) then degassed for 10 mm. Pd(dppf)C12.CH2CI2 (445 mg, 0.545 mmol) was added then the mixture was degassed for a further 5 mm. The reaction was heated at 100 C for 18 h then allowed to cool to RT. The reaction mixture was filtered then the collected solids were washed with EtOAc (50 ml). The combined filtrate wasconcentrated in vacuo. The residue was re-dissolved in EtOAc:heptane (1:1) then filtered through a silica pad. The pad was rinsed with EtOAc:heptane (1:1, 200 ml). The filtrate was concentrated in vacuo to afford an off-white solid (3.94 g). The silica pad was rinsed through further with EtOAc (200 ml) to afford a brown solid (1.68 g). The brown solid from the EtOAc filtrate was pre-adsorbed onto silica, then purified by flash columnchromatography on a silica column (50 g). The column was eluted with EtOAc:heptane, using the following gradient (%EtOAc, column volumes): 0%, 1 CV; 0-30%, 11 CV; 30%, 20 CV; 30-45%, 4.5 CV; 45%, 7.5 CV; 45-50%, 1 CV; 50%, 15 CV. The desired fractionswere combined and concentrated in vacuo to afford an off-white solid (1.00 g, 21%).1H NMR (500 MHz, DMSO-d6) O 7.67 (d, J= 8.2 Hz, 2H), 7.59 (d, J= 8.2 Hz, 2H), 7.42(d, J= 8.2 Hz, 2H), 7.28 (d, J= 8.1 Hz, 2H), 6.90 (t, J= 5.5 Hz, 1H), 4.07 (5, 2H), 3.17(q, J = 6.5 Hz, 2H), 2.73 (t, J = 7.4 Hz, 2H), 1.44 – 1.29 (m, 9H).LC/MS (System A): R = 1.27 mi UV purity = 97%.

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, N-Boc-2-(4-Bromophenyl)ethylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ENTERPRISE THERAPEUTICS LIMITED; HAY, Duncan, Alexander; SCHOFIELD, Thomas, Beauregard; WENT, Naomi; MCCARTHY, Clive; (108 pag.)WO2019/77340; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 13304-62-6, name is N-Benzylacrylamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: N-Benzylacrylamide

General procedure: To a solution of 3-iodo-chromone (4 mmol) and olefin (4.8 mmol) in solvent was added catalyst (5 mmol %) and base (8 mmol). The reaction mixture was stirred via microwave heating under air. Then the mixture was poured into 10% HCl ice-water (300 mL) slowly with stirring. The suspension was filtered through a filter and filter cake was collected and dried. The crude product was purified by chromatography over silica gel to give resulting product.

The synthetic route of 13304-62-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Yikai; Lv, Zhiliang; Zhong, Hanyu; Zhang, Mingfeng; Zhang, Tao; Zhang, Wannian; Li, Ke; Tetrahedron; vol. 68; 47; (2012); p. 9777 – 9787;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 108966-71-8, 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. 108966-71-8, name is 3,4-Difluorobenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 500 mL round-bottomed flask fitted with a condenser and N2 inlet septum was placed a stir bar, 3, 4-difluoro-benzenesulfonamide (10 g, 52 mmol), anhydrous hydrazine (10. 56 mL, 336 mmol), and acetonitrile (180 mL). The mixture was refluxed for 6 h under N2. The solvent was then removed under vacuum and the residue was treated with H2O. The separated solid was filtered and washed with H20 to give the desired product. Exact mass calculated for C6H8FN302S 205. 03, found 206. 1 (MH+).

The synthetic route of 3,4-Difluorobenzenesulfonamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARENA PHARMACEUTICALS, INC.; WO2005/7658; (2005); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

617-36-7, name is Ethyl 2-amino-2-oxoacetate, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: Ethyl 2-amino-2-oxoacetate

4′-Nitro-2-bromoacetophenone (6.100 g, 25 MMOL) and ethyl thioxamate (3.460 g, 26 MMOL) were dissolved in MeOH (20 mL) and the solution was refluxed for 1 h. After cooling to room temperature, the precipitated solid was collected by filtration, washed with cold MEOH and dried under vacuum (5.15 g, 75% yield).

The synthetic route of 617-36-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO KG; WO2004/65367; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 869494-16-6, name is tert-Butyl 3,6-diazabicyclo[3.1.1]heptane-6-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C10H18N2O2

A mixture of (R)-4-(6-fluoropyridin-3 -yl)-6-(2-hydroxypropoxy)pyrazolo[ 1,5 – a]pyridine-3-carbonitrile (Intermediate P66; 100 mg, 0.320 mmol) 3,6-diaza- bicyclo[3.1.1]heptane-6-carboxylic acid tert-butyl ester (95.2 mg, 0.480 mmol) and K2C03(s) (443 mg, 3.20 mmol) in DMSO (1601 tL) was stirred for 3 d at 80 °C. The reaction mixture was cooled to ambient temperature, then diluted with water (10 mL), and extracted with DCM (4 x 10 mL). The combined organic extracts were washed with brine (10 mL), then dried over anhydrous Na2SO4(), filtered, and concentrated in vacuo. The crude residue was purified by silica chromatography (using 50-100percent EtOAc in Hexanes as the gradient eluent) to cleanly provide the title compound (97 mg, 62percent yield). MS (apci) m/z = 491.2 (M+H).

According to the analysis of related databases, 869494-16-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ANDREWS, Steven W.; ARONOW, Sean; BLAKE, James F.; BRANDHUBER, Barbara J.; COOK, Adam; HAAS, Julia; JIANG, Yutong; KOLAKOWSKI, Gabrielle R.; MCFADDIN, Elizabeth A.; MCKENNEY, Megan L.; MCNULTY, Oren T.; METCALF, Andrew T.; MORENO, David A.; TANG, Tony P.; REN, Li; (668 pag.)WO2018/71447; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide, A new synthetic method of this compound is introduced below., Recommanded Product: 830-43-3

EXAMPLE 159 Synthesis of 1-(2-chlorobenzyl)-2-methyl-6-[4-(trifluoromethyl)benzenesulfonylcarbamoyl]benzimidazole (221) In the same manner as in Example 158, 0.390 g of 1-(2-chlorobenzyl)-2-methyl-6-[4-(trifluoromethyl)benzenesulfonylcarbamoyl]benzimidazole (221) were formed from 0.450 g of 6-carboxy-1-(2-chlorobenzyl)-2-methylbenzimidazole, 0.486 g of N,N’-carbonyldiimidazole, 0.676 g of 4-(trifluoromethyl)benzenesulfonamide and 0.457 g of diazabicycloundecene.

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; Fujisawa Pharmaceutical Co., Ltd.; US6166219; (2000); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 143557-91-9, 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. 143557-91-9, name is tert-Butyl 3-endo-3-hydroxy-8-azabicyclo[3.2.1]octane-8-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Triphenylphosphine (3.57 g, 13.6 mmol) was solved in toluene (40 ml) and cooled to <;20C. Diethylazodicarboxylate (40% in toluene) (6.2 ml, 13.6 mmol) was added to the mixture below 20C, followed by stirring for 10 minutes, endo-3- Hydroxy-8-aza-bicyclo[3.2.1] octane-8-carboxylic acid te/t-butyl ester (2.58 g, 11.3 mmol) was added and after 10 minutes 7-hydroxy-3-methyl-chromen-2-one (2.0 g, 11.3 mmol) was added to the mixture. The temperature raised to 28C due to an exothermic reaction. The mixture was allowed to stir for 15 h at room temperature. Water (50 ml) and sodium hydroxide (20 ml, 0.1 M) was added followed by stirring. The mixture was filtered and washed with water and diethylether. Yield 2.50 g (57%). The chemical industry reduces the impact on the environment during synthesis tert-Butyl 3-endo-3-hydroxy-8-azabicyclo[3.2.1]octane-8-carboxylate. I believe this compound will play a more active role in future production and life. Reference:
Patent; NEUROSEARCH A/S; PETERS, Dan; NIELSEN, Elsebet, Østergaard; NIELSEN, Karin, Sandager; MUNRO, Gordon; WO2010/130620; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 116861-31-5, name is tert-Butyl (3-chloropropyl)carbamate, molecular formula is C8H16ClNO2, 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. SDS of cas: 116861-31-5

[2-Amino-6-(4,5-difluoro-2-hydroxymethylphenyl)quinazolin-4-yl]-(1,3-dihydroisoindol-2-yl)methanone (?A64?) [0665] 100 mg of [2-amino-6-(4,5-difluoro-2-hydroxymethylphenyl)quinazolin-4-yl]-(1,3-dihydroisoindol-2-yl)methanone are dissolved in 3 ml of tetrahydrofuran together with 90 mg of tert-butyl (3-chloropropyl)carbamate. 2 ml of sodium hydroxide solution (32%) and 2 mg of tetrabutylammonium iodide are added, and the mixture is stirred at 80 C. for 16 h. The mixture is extracted 3 times with 5 ml of ethyl acetate. The combined organic phases are dried over sodium sulfate. After filtration, the filtrate is evaporated to dryness, the residue is taken up in 3 ml of dichloromethane, and 1 ml of 4N HCl in dioxane is added. After 1 h at 25 C., the mixture is evaporated to dryness in vacuo and purified by chromatography (reversed phase HPLC). [0666] Yield: 18 mg (16%) of {2-amino-6-[2-(3-aminopropoxymethyl)-4,5-difluorophenyl]quinazolin-4-yl}-(1,3-dihydroisoindol-2-yl)methanone; [0667] LC-MS retention time: 1.66 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 116861-31-5, its application will become more common.

Reference:
Patent; MERCK PATENT GESELLSCHAFT MIT BESCHRANKTER HAFTUNG; Eggenweiler, Hans-Michael; Sirrenberg, Christian; Buchstaller, Hans-Peter; US2013/178443; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 88-96-0, name is Phthalamide, A new synthetic method of this compound is introduced below., Computed Properties of C8H8N2O2

To a solution of (S)-tert-butyl 4-(3-(l-hydroxyethyl)benzyl)piperazine-l- carboxylate (480 mg, 1.50 mmol) in 10 mL of anhydrous THF at 00C under a positive pressure of N2 were added phthalimde (330 mg, 2.25 mmol), triphenyl phosphine (590 mg, 2.25 mmol) and DIAD (440 DL, 2.25 mmol). The solution was warmed up to ambient temperature and stirred 1 h. The solvent was removed at reduced pressure and the residue was purified by reverse-phase HPLC to afford (S)-rerr-butyl 4-(3-(l-(l,3-dioxoisoindolin-2- yl)ethyl)benzyl)piperazine-l-carboxylate as 490 mg of a white solid.

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; CYTOKINETICS, INC.; WO2007/89336; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics