Tag: M.W=200-300

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. 49834-22-2, name is 3-Bromo-N-methylbenzamide, A new synthetic method of this compound is introduced below., Recommanded Product: 3-Bromo-N-methylbenzamide

200 mg of tetrakistriphenylphosphine palladium was added under cooling with ice to a solution of 0.86 g of N-methyl-3-bromobenzamide in a mixed solvent of 10 ml of toluene and 3 ml of ethanol, followed by stirring for 20 minutes. 0.93 g of 4-chloro-2,6-dimethylbenzene boronic acid and 4.5 ml of a 2M sodium carbonate aqueous solution were added thereto, and the reaction system was flushed with nitrogen, followed by reflux under heating for 9 hours. After cooling, 50 ml of cold water was added, and then, 50 ml of ethyl acetate was added. The precipitate was filtered off. Then, the organic layer was separated from the filtrate. The water layer was extracted again with 50 ml of ethyl acetate. The organic layers were put together and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel (Silica gel 60N; spherical and neutral, manufactured by Kanto Kagaku) column chromatography (developing solvent of n- hexane: ethyl acetate=1 : 1) to obtain 0.40 g of the objective compound having a melting point of 137. 1C. Further, NMR of this compound was as follows. 1H-NMR 5 (ppm) 1.98 (s, 6H), 3.02 (d, 3H; J =5. 1 Hz), 6.18 (bs, lH), 7.10 (s, 2H), 7.24 (d, lH ; J =7. 5 Hz), 7.49 (t, lH; J =7. 5 Hz), 7.51 (s, lH), 7.75 (d, lH; J =7. 5 Hz)

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; ISHIHARA SANGYO KAISHA, LTD.?; WO2005/44007; (2005); A1;,
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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. 535170-20-8, name is tert-Butyl (3-amino-2,6-difluorophenyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of tert-Butyl (3-amino-2,6-difluorophenyl)carbamate

The tert-butyl-3-amino-2,6-difluorophenylcarbamate (50 mg, 0.20 mmol) prepared at Step 3 was added and dissolved into dichloromethane solvent. 1-methyl-1H-imidazole-4-sulfonyl chloride (44 uL, 0.25 mmol) and pyridine (50 uL, 0.61 mmol) were added into the reaction solution and stirred at 50C for 2 hours. After the reaction, the reactant was washed with 1N aqueous hydrochloric acid solution and salt water. After extraction with dichloromethane, the organic layer was dried with sulfuric anhydride magnesium and vacuum concentrated, and then refined by means of column chromatography, so that 74 mg of the target compound, tert-butyl-2,6-difluoro-3-(1-methyl-1H-imidazole-4-sulfonamido)phenylcarbamate (percentage yield: 95%), was obtained.1H NMR(400MHz, DMSO-d6) : delta 9.96(bs, 1H), 8.82(s, 1H), 7.78(s, 1H), 7.68(s, 1H), 7.17(m, 1H), 7.03(m, 1H), 3.25(s, 3H), 1.40(s, 9H).

The synthetic route of 535170-20-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Youai Co., Ltd.; SHIM, Eun Kyong; KIM, Nam Doo; SHIM, Tae Bo; KIM, Seung Yong; EP2647637; (2013); A2;,
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Some common heterocyclic compound, 40724-47-8, name is 4-Bromomethylbenzenesulfonamide, molecular formula is C7H8BrNO2S, 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. Formula: C7H8BrNO2S

Exam le 81 4-(azidomethy 3 )benzen esul fonam id e To a stirred solution of 4-(bromomethyl)benzenesulfonamide (0.50 g) in N,Ar-dimethylformarnide (ImL) was added sodium azide (0.20 g). The suspension was heated to 50C for 3 hours at which points the solvent was removed under reduced pressure. The residue was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over magnesium sulfate, filtered and concentrated to dryness to give the title compound as a syrup that solidified on standing. NM (400 MHz, Chioroforn ) delta 8.06 — 7.91 ( rn. 2H), 7.58 FontWeight=”Bold” FontSize=”10″ – 7.44 (m, 2H), 4.96 is, 2H), 4.48 (s, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 40724-47-8, its application will become more common.

Reference:
Patent; THE CENTRE FOR DRUG RESEARCH AND DEVELOPMENT; WINTERS, Geoffrey C.; MANDEL, Alexander Laurence; RICH, James R.; HEDBERG, Bradley John; HSIEH, Tom Han Hsiao; BOURQUE, Elyse Marie Josee; BABCOOK, John; WO2014/144871; (2014); A1;,
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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. 24167-51-9, name is 3-Bromo-N,N-dimethylbenzamide, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 24167-51-9

General procedure: The following experimental procedure for the chemoselective partial reduction of ethyl benzoate and N,N-dimethyl 3-toluamide is representative. A dry and argon-flushed flask, equipped with a magnetic stirring bar and a septum, was charged with ethyl benzoate (0.07mL, 0.5mmol), N,N-dimethyl 3-toluamide (0.08mL, 0.5mmol) and 5mL THF. After CDBBA (9.01mL, 0.44M soln. 4.0mmol) was slowly added and stirred for 12h at room temperature. The reaction was quenched by aqueous 1N HCl (10mL) and extracted with diethyl ether (2¡Á10mL). The combined organic layers were dried over MgSO4. GC analysis showed a 97% recovery yield of ethyl benzoate and 95% yield of 3-methylbenzaldehyde. All products in Table 2 were confirmed through comparison with GC data of authentic sample.

According to the analysis of related databases, 24167-51-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Im, So Hee; Shin, Won Kyu; Jaladi, Ashok Kumar; An, Duk Keun; Tetrahedron Letters; vol. 59; 24; (2018); p. 2335 – 2340;,
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Related Products of 85006-25-3, The chemical industry reduces the impact on the environment during synthesis 85006-25-3, name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate, I believe this compound will play a more active role in future production and life.

Example 29: 2-r i -r2,5-difluoro-4-rr(3,S,,6R)-3-methyl-l,l-dioxo-6-phenyl-thiazinan-2- Step 1: ferf-Butyl ((ferf-butoxycarbonyl)oxy)(l-(2,5-difluoro-4-(((3^,6R)-3-methyl-l,l-dioxido-6-phenyl- l,2-thiazinan-2-yl)methyl)phenyl)ethyl)carbamate To a solution of l-(2,5-difluoro-4-(((35′,6R)-3-methyl-l,l-dioxido-6-phenyl-l,2-thiazinan-2- yl)methyl)phenyl)ethyl methanesulfonate (500 mg, 1.1 mmol) in acetonitrile (30 mL) was added tert- butyl ferf-butoxycarbonyloxycarbamate (492 mg, 2.1 mmol) and Cs2C03 (1 g, 3.1 mmol). The mixture was stirred at 130 C for 3 h. The solid was removed by filtration and the filtrate was evaporated. The resulting residue was purified by Biotage Flash column (20 g silica, UV254, PE/EA= 1:0-2: 1) to afford the title compound (363 mg, 50% yield) as a white solid. LCMS (ESI): m/z = 633.0 [M+Na]+.

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, tert-Butyl (tert-butoxycarbonyl)oxycarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; FAUBER, Benjamin; LADDYWAHETTY, Tammy; RENE, Olivier; (105 pag.)WO2016/96936; (2016); A1;,
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Electric Literature of 142-78-9, 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. 142-78-9, name is N-(2-Hydroxyethyl)dodecanamide, This compound has unique chemical properties. The synthetic route is as follows.

33 mg (4.5 mol %) of KBr (co-catalyst) was dissolved in 6 mL of water. Tetrahydrofuran solvent THF (31 mL), AA-TEMPO catalyst (25 mg, 2.5 mol %) and 1.5 g N-lauroylethanolamide (LMEA) were added with stirring to give a homogeneous water-white solution. Sodium hypochloride oxidizing agent (22 mL of 11.5% aq. Solution, 6.5 equivalents) and 2.3 mL of 2 NaOH (to maintain pH above 7) were mixed. The combined solution was added dropwise to the solution of LMEA and catalyst over a period of 1.5 hour. A separate aqueous layer immediately formed upon addition of the sodium hypochlorite solution. The pH of the aqueous layer was 12.7 after addition of the first 3.5 ml. The temperature was maintained below 32 C. with an ice-water bath. The reaction was stirred for 0.5 hr. more until complete conversion of LMEA to LG as determined by reversed-phase High Pressure Liquid Chromatography, abbreviated HPLC. The pH at end of the reaction was 7.6.At completion of the reaction, the mixture was acidified to pH 3.0 (to get the purified carboxylic acid) by addition of 8.5 mL of 1 N HCl, and the layers were separated. The lower aqueous layer was extracted with 30 mL THF, and the combined THF layers were concentrated on a rotary evaporator and dried in vacuo to give N-lauroylglycine in 116% yield (residual water present); Example 2 Oxidation of LMEA with 3.25 eq. of NaOCl, and Acid Work-UpThe procedure in Example 1 was followed, except that the amount of sodium hypochlorite was decreased to 3.25 equivalents. The isolated yield was 103% (includes residual water), showing that the oxidation works with the lower sodium hypochlorite amount; Example 4Oxidation of LMEA in THF with 6.5 eq. of NaOCl, Drowning Procedure at pH=2.6The procedure of Example 1 was followed except for the isolation step. After completion of the reaction, the mixture was acidified to pH=2.6 with 9.25 mL of 1 N HCl. The entire reaction mixture (both THF and water phases) were poured in 240 mL of water with vigorous stirring. The precipitated product was isolated by gravity filtration, and washed with 200 mL water. After air-drying, and further drying in vacuo, the product was obtained in 77% yield. The yield can be improved by better filtration techniques, e.g. by pressure filtration through a 0.45 mum or less filter; Example 5Oxidation of LMEA in THF with 3.25 eq. of NaOCl, Drowning Procedure, Effect of pH on YieldThe procedure of Example 2 was followed except for the isolation step. After completion of the reaction, the mixture was only partially acidified (to pH=5.2 with 3.6 mL of 1 N HCl.) The entire reaction mixture (both THF and water phases) were poured in 240 mL of water with vigorous stirring. The precipitated product was isolated by gravity filtration, and washed with 240 mL water. After drying in vacuo overnight, the product was obtained in 59% yield (based on free carboxylic acid), and 55% (based on the sodium carboxylate). The lower yield than Example 4 is attributed to the larger proportion of the water-soluble sodium carboxylate at the higher pH.

The chemical industry reduces the impact on the environment during synthesis N-(2-Hydroxyethyl)dodecanamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Conopco, Inc.; US7307187; (2007); B1;,
Amide – Wikipedia,
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Electric Literature of 4943-86-6, 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. 4943-86-6, name is 2-Amino-N-(4-chlorophenyl)benzamide, This compound has unique chemical properties. The synthetic route is as follows.

The reaction flask was added 1l (2mmol, 493mg),and then added tert-butyl nitrite (6mmol, 0.72mL),followed by tetrabutylammonium iodide (5mol%,37 mg of) and acetonitrile (20mL). Then the system was heated for 12 hours at 60 deg C. for air, vacuum spin dry acetateAfter the nitrile with petroleum ether / ethyl acetate = 6/1 mixed solvent of a simple column chromatography to give the product 2L, 86% yield. yellowsolid,

The chemical industry reduces the impact on the environment during synthesis 2-Amino-N-(4-chlorophenyl)benzamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Zhengzhou Institute of Light Industry; Yan, Yi zhe; Shi, Miao miao; Liu, Yan qi; Zhi, Huan huan; He, Yuan; Niu, Bin; (18 pag.)CN105418525; (2016); A;,
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Adding a certain compound to certain chemical reactions, such as: 180079-94-1, name is tert-Butyl 3-aminophenethylcarbamate, belongs to amides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 180079-94-1, Formula: C13H20N2O2

Production Example 30 Production of 3′,4′-dihydro-2’H-spiro[cyclobutane-1,1′-isoquinolin]-6′-amine 2 mL of 85 % phosphoric acid was added to 350 mg of the compound obtained in Production Example 29-2), and stirred at 70C for 1 hour. Further, 0.144 mL of cyclobutanone was added to it, and reacted at 140C for 3 hours, using a microwave reactor. The reaction liquid was diluted with water, then potassium carbonate was added to it, and extracted with ethyl acetate. This was washed with saturated saline water, dried with anhydrous magnesium sulfate, and the solvent was evaporated away. The crude product was purified through basic silica gel column chromatography (hexane/ethyl acetate) to obtain 157 mg of the entitled compound as a colorless oily compound. 1H-NMR (CDCl3) delta: 7.28 (1H, d, J=8.3 Hz), 6.59 (1H, dd, J=8.3, 2.9 Hz), 6.37 (1H, d, J=2.4 Hz), 3.54 (2H, s), 3.03 (2H, t, J=5.9 Hz), 2.68 (2H, t, J=6.1 Hz), 2.47-2.40 (2H, m), 2.18-2.07 (3H, m), 2.02-1.92 (1H, m)

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, tert-Butyl 3-aminophenethylcarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Banyu Pharmaceutical Co., Ltd.; EP2168966; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6325-93-5, name is 4-Nitrobenzenesulfonamide, belongs to amides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 6325-93-5, HPLC of Formula: C6H6N2O4S

General procedure: A mixture of nitroarene (1 mmol), PdCu/graphene (6 mg) and sodium borohydride (2 mmol) were taken in a 25 mL reaction tube. 3 mL of EtOH:H2O (1:2 in volume ratio) was added by a syringe at 0 C. After 10 min the reaction mixture was placed in an oil bath at 50 C. The reaction was monitored by TLC. On completion, the reaction mixture was extracted with ethylacetate and dried ove ranhydrous Mg2SO4. Evaporation of the combined organic layer andfollowed by column chromatography over silica gel (60-120 mesh) afforded desired corresponding amines.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Feng, Yi-Si; Ma, Jing-Jing; Kang, Yu-Mei; Xu, Hua-Jian; Tetrahedron; 36; (2014); p. 6100 – 6105;,
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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. 85006-25-3, name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 85006-25-3

To a suspension of sodium hydride (60% in mineral oil, 10 mg, 0.250 mmol) in 0.5 mL of DMF , N,O-diBoc-hydroxylamine (55.6 mg, 0.230 mmol) was added. The mixture was stirred for 30′ at 0C then a solution of 3-[3′- Adamantan-1 -yl-4′-(2-bromo-ethoxy)-biphenyl-4-yl]-acrylic acid ferf-butyl ester (103 mg, 0.192 mmol) in 2 mL of DMF was slowly added. After having stirred at room temperature overnight, DMF was evaporated, the residue was poured into saturated solution of NH4CI and extracted with ethyl acetate. The organic phase was dried and evaporated. Purification by flash chromatography (Hexane/Ethyl acetate 90:10) gave 109 mg (81 %) of the desired compound as white solid; m.p. 165C, Rf(Hexane/Ethyl acetate 90:10) 0.26.1H-NMR (300 MHz, CDCI3) delta:7.61 (1 H, d, J = 16.1 Hz); 7.57.7.50 (4H, m); 7.47 (1 H, d, J = 2.21 Hz); 7.39 (1 H, dd, J = 8.46, 2.21 Hz); 6.93 (1 H, d, J = 8.46 Hz); 6.38 (1 H, d, J = 16.1 Hz); 4.27-4.17 (2H, m); 4.16-4.01 (2H, m); 2.22-2.02 (9H, m), 1 .86- 1 .70 (6H, m), 1 .54 (9H, s); 1 .52 (9H, s); 1.49 (9H, s).

The synthetic route of 85006-25-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOGEM S.CA.R.L.; PISANO, Claudio; DALLAVALLE, Sabrina; CINCINELLI, Raffaella; MERLINI, Lucio; (56 pag.)WO2018/60354; (2018); A1;,
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