Month: July 2021

Some common heterocyclic compound, 72505-21-6, name is 4-(Trifluoromethyl)thiobenzamide, molecular formula is C8H6F3NS, 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. Computed Properties of C8H6F3NS

Step B 2-(4-Trifluoromethylphenyl)thiazole A stirred solution of 5.0 grams (0.024 mole) of 4-trifluoromethylbenzthioamide, 4.4 grams (0.026 mole) of bromoacetaldehyde dimethyl acetal, and 4 drops of concentrated hydrochloric acid in 50 ml of ethanol was heated at reflux for 18 hours. After this time the reaction mixture was subjected to column chromatography on silica gel. Elution was accomplished using 20% ethyl acetate in hexane. The appropriate fractions were combined and concentrated under reduced pressure, yielding 3.3 grams of 2-(4-trifluoromethylphenyl)thiazole. The nmr spectrum was consistent with the proposed structure.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 72505-21-6, its application will become more common.

Reference:
Patent; FMC Corporation; US5073564; (1991); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 147751-16-4, These common heterocyclic compound, 147751-16-4, name is tert-Butyl methylsulfonylcarbamate, 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.

Boc-N-methanesulfonamide (11.0 g, 56.3 mmol), trimethylphosphine (56.1 mL of a 1.0 M solution in tetrahydrofuran, 56.1 mmol), and a 40 wt. % solution of diethyl azodicarboxylate in toluene (25.6 mL, 56.0 mmol) were added sequentially to a solution of (4-benzylsulfanyl-5-nitro-thiophen-3-yl)-methanol (10.52 g, 37.4 mmol) in tetrahydrofuran (300 mL) at 25 C. The mixture was stirred for 3.5 h at 25 C., and then was concentrated in vacuo. Purification of the residue by flash column chromatography (Merck silica gel 60, 40-63 mum; 20% ethyl acetate in hexanes) afforded the desired product, Boc-N-(4-benzylsulfanyl-5-nitro-thiophen-3-ylmethyl)-methanesulfonamide (9.79 g, 21.3 mmol, 57%), as a dark brown oil. 1H NMR (400 MHz, CDCl3) delta: 1.50 (9H, s), 3.29 (3H, s), 4.19 (2H, s), 4.68 (2H, s), 7.15-7.18 (2H, m), 7.22-7.25 (3H, m), 7.40 (1H, s).

The synthetic route of 147751-16-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anadys Pharmaceuticals, Inc.; US2012/316156; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 183059-24-7,Some common heterocyclic compound, 183059-24-7, name is tert-Butyl 2-hydroxy-2-methylpropylcarbamate, molecular formula is C9H19NO3, 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.

To a mixture of intermediate 16 (3.0 g, 15.9 mmol, crude) in anhydrous DCM (50 mL) was added DAST (2.3 mL, 17.4 mmol) at -78 C under a nitrogen atmosphere. The mixture was stirred at -78 C for 1 h, and allowed to warm to rt overnight. The mixture was then cooled to 0 C, and quenched by addition of saturated aqueous layer NaHCO3(30 mL) with stirring at 0 C slowly. The mixture was separated, and the aqueous layer was extracted with DCM (2x 20 mL). The combined organic layers were washed with brine (2 x 30 mL), dried, filtered and concentrated under vacuum to give the crude intermediate 17 (2.5 g, 76% crude), which was used directly in next step without purification. 1H NMR: (CDCI3): delta 4.82 (br, 1H), 3.30-3.35 (d, = 6.0 Hz, 1H), 3.24-3.26 (d, = 6.0 Hz, 1H), 1.44 (s, 9H), 1.37 (s, 3H), 1.35 (s, 3H).19F NMR: (CDC13400 MHz): delta -144.93.

The synthetic route of 183059-24-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; VITAE PHARMACEUTICALS, INC.; BUKHTIYAROV, Yuri; CACATIAN, Salvacion; DILLARD, Lawrence, Wayne; DORNER-CIOSSEK, Cornelia; FUCHS, Klaus; JIA, Lanqi; LALA, Deepak, S.; MORALES-RAMOS, Angel; RAST, Georg; REEVES, Jonathan; SINGH, Suresh, B.; VENKATRAMAN, Shankar; XU, Zhenrong; YUAN, Jing; ZHAO, Yi; ZHENG, Yajun; WO2013/134085; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 85006-25-3, A common heterocyclic compound, 85006-25-3, name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate, molecular formula is C10H19NO5, 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.

General procedure: Nucleophile (1-3 mol equiv), tris-(dibenzylideneacetone)dipalladium (2.5 mol %), tris-(2-furyl)phosphine (10 mol %) and potassium carbonate (2 mol equiv) were added to a solution of the aryl halide (1 mmol) in dry dimethylformamide (10 mL) in a Schlenk tube. The reaction mixture was then degassed using the freeze, pump, thaw (F.P.T.) technique (one cycle). Allene gas was then introduced at the required pressure (1 atm) and the Schlenk tube contents stirred and heated at 80 C for 16 h. After cooling and venting, DCM (20 mL) was added and the mixture filtered to remove inorganic salts. The filtrate was concentrated in vacuo and the residue was purified by column chromatography.

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:
Article; Elboray, Elghareeb E.; Gao, Chuanjun; Grigg, Ronald; Tetrahedron; vol. 68; 14; (2012); p. 3103 – 3111;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 62009-47-6, The chemical industry reduces the impact on the environment during synthesis 62009-47-6, name is 2-Aminomalonamide, I believe this compound will play a more active role in future production and life.

EXAMPLE 10 In 2.1 mL of water is suspended 0.5 g of 2-aminomalonamide. Under ice-cooling, 0.43 g of ethyl glyoxalate is added to the suspension, which is then stirred for 40 minutes. Then, 0.85 mL of 5 mol/mL sodium hydroxide is added to the resulting suspension, which is then stirred at the same temperature as above for 40 minutes. The reaction mixture is adjusted to pH 12 by adding 1 mol/L sodium hydroxide, and once made into a solution. The solution is then adjusted to pH 2 by adding 6 mol/mL hydrochloric acid. The deposited crystals are collected by filtration and washed successively with water and 50% (w/w) ethanol to obtain 0.15 g of 3,5-dihydroxy-2-pyrazinecarboxamide. IR(KBr) cm-1: 1660 NMR(D2O) delta value: 6.97(1H,s)

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, 2-Aminomalonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Furuta, Yousuke; Egawa, Hiroyuki; Nomura, Nobuhiko; US2002/13316; (2002); 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. 563-83-7, name is Isobutyramide, A new synthetic method of this compound is introduced below., Application In Synthesis of Isobutyramide

General procedure: Acetone (5.0 mL) was added to the mixture of amide (2.0 mmol) and aldehyde (1.0mmol), followed by the addition of BF3 etherate (12.6 muL, 0.1 mmol).Then the mixture was stirred at room temperature until the full consumption ofstarting material detected by TLC analysis. Then the product was collected assolid by filtration and washed with a small portion of diethyl ether. After drying under vacuum, the purity was checked by 1HNMR: only desired peaks were observed except minor solvent residue in only afew cases.

The synthetic route of 563-83-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Yi; Zhong, Zhihao; Han, Yingmei; Han, Ruirui; Cheng, Xu; Tetrahedron; vol. 69; 52; (2013); p. 11080 – 11083;,
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. 4141-08-6, name is 2-Amino-N-methylbenzamide, A new synthetic method of this compound is introduced below., Formula: C8H10N2O

General procedure: For the 5-subsititution was H, F or Cl, the procedure was as follows: A mixture of compound 7 (0.79 g, 5.25 mmol), 5-substituted-2,4-dichloropyrimidine (5 mmol) and DIPEA (1.05 mL,6 mmol) in i-PrOH was heated under reflux for 6 h.Water (100 mL)was added and the solid was filtered off, washed with water and driedto obtain compounds 10a-10c. For the 5-subsititution was methyl or methoxy, the procedure was as follows: To a mixture of compound 7 (1.26 g, 8.4 mmol) and5-substituted-2,4-dichloropyrimidine (8 mmol) was added NaH (60%, 0.38 g, 9.6 mmol) in DMF (6 mL) under ice bath. Then the mixture was stirred for 24 h at room temperature.Water was added dropwise to stop the reaction. The reaction mixture was extracted withdichloromethane (20 mL x 3), and the combined organic layer waswashed with brine (15mL x 2), dried over anhydrous Na2SO4 and concentrated under vacuum to afford the crude product. The residue was purified by column chromatography to obtain compound 10d and 10e.

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:
Article; Su, Yue; Li, Ridong; Ning, Xianling; Lin, Zhiqiang; Zhao, Xuyang; Zhou, Juntuo; Liu, Jia; Jin, Yan; Yin, Yuxin; European Journal of Medicinal Chemistry; vol. 177; (2019); p. 32 – 46;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 40545-33-3, These common heterocyclic compound, 40545-33-3, name is 2-Amino-5-methylbenzamide, 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.

General procedure: A 15 mL tube was added 2-aminobenzamide (1 mmol), benzyl amine (1.5 mmol), and a stir bar. Then H2O2 (30 wt% in H2O, 5 equiv.) was added by a syringe at room temperature under open air. The tube was closed and kept at 120C for 20 h. The conversion and yield were determined by GC and GC-MS using hexadecane (0.1 mmol) as the internal standard.

Statistics shows that 2-Amino-5-methylbenzamide is playing an increasingly important role. we look forward to future research findings about 40545-33-3.

Reference:
Article; Qi, Xin-Xin; Song, Zhen-Zhen; Gong, Jin-Long; Fang, Zheng-Yu; Wu, Xiao-Feng; Chinese Chemical Letters; vol. 27; 1; (2016); p. 21 – 24;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 617-36-7, The chemical industry reduces the impact on the environment during synthesis 617-36-7, name is Ethyl 2-amino-2-oxoacetate, I believe this compound will play a more active role in future production and life.

Step 1: Preparation of N-(2,2,6,6-tetramethyl-4-piperidinyl)oxamide Into a 3-neck, 250 ml, round bottom flask was added 30.5 g (0.25 mole) of ethyl oxamate (Aldrich Chemical Company) and 100 ml of methanol. The flask was equipped with a magnetic stirrer, thermometer, reflux condenser and addition funnel containing 39.0g (0.25 mole) 4-amino-2,2,6,6-tetramethylpiperidine. The stirrer was activated and the amine was added dropwise to the ethyl oxamate solution over 12 minutes as the temperature slowly rose to 35C. The reaction was stirred an additional 2.5 hours and filtered. After air drying overnight, the filter cake weighed 40.4g and had a melting point of 203-208C. The filtrate was transferred back to the 250 ml 3-neck flask and another 30.5g of ethyl oxamate was added. An additional 39g of 4-amino-2,2,6,6-tetramethylpiperidine were added over 7 minutes as the temperature slowly rose to 28C. The reaction was stirred 3 hours and filtered. After air drying overnight, the filter cake weighed 50.0g and had a melting point of 198-200C. The infrared spectrum (nujol mull) of the product contained a sharp NH band at 3370 cmmin1, a strong broad carbonyl band at 1670 cmmin1 and a weaker carbonyl band at 1520 cmmin1.

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, Ethyl 2-amino-2-oxoacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ELF ATOCHEM NORTH AMERICA, INC.; EP516192; (1992); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 13304-62-6, 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. 13304-62-6, name is N-Benzylacrylamide, This compound has unique chemical properties. The synthetic route is as follows.

The preparation method is as follows: Add a N-benzyl acrylamide dioxane solution to a clean 30 mL round bottom flask with stirring magnets at a concentration of 1 M. Then adding the catalyst cerium acetate (10 mol%), Oxidant silver carbonate (3 eq), additive potassium hexafluorophosphate (0.5 eq), 1,2-diphenylacetylene (1.0 eq). This mixture was stirred at room temperature for one hour and then heated to reflux overnight. The reaction was detected by thin plate chromatography, and after the reaction was completed, it was cooled to room temperature, and the reaction was quenched with water. Extract 4×20 mL with ethyl acetate and wash with saturated brine. Dry over anhydrous sodium sulfate and remove sodium sulfate by filtration. The solvent was evaporated under reduced pressure to give a crude material. Using petroleum ether/ethyl acetate as the eluent, Purified by column chromatography (mobile phase: ethyl acetate / petroleum ether = 1/2) A pale yellow solid product was obtained in a yield of 60%.

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

Reference:
Patent; Lanzhou University; Li Yumin; Chen Hao; Han Zhijian; (27 pag.)CN109928969; (2019); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics