Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 78191-00-1, name is N-Methoxy-N-methylacetamide, 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 78191-00-1, Recommanded Product: 78191-00-1

5-methyl-thiazole (2.00g, 20.2mmol) was dissolved in tetrahydrofuran (50 mL) , at -78C, under nitrogen gas protection was slowly added dropwise n-butyl lithium (2.5M in tetrahydrofuran, 9.68mL, 24.2mmol). The reaction solution was stirred for 0.5 hours at -78C, and dissolved in tetrahydrofuran was slowly added dropwise (ImL) of N- methoxy -N- methyl-acetamide (2.50g, 24.2mmol). The reaction was warmed to 0C stirred for 1.5 h. At 0C slow addition of water (10mL) to the reaction mixture, and extracted with ethyl acetate(30mLx3) . The combined organic phase was dried over anhydrous sodium sulfate, filtered, and evaporated under reduced pressure, the obtained product was purified by preparative high performance liquid chromatography (1: 1 petroleum ether / ethyl acetate, Rf = 0.7) to give the product 1-(5-methylthiazol-2-yl)ethanone (1.45 g of, as a yellow solid), yield: 51%.

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-Methoxy-N-methylacetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sichuan Gooddoctor Pharmaceutical Group Co., Ltd.; Wu, Lingyun; Zhang, Peng; Zhang, Li; Li, Jian; Chen, Shuhui; Geng, Funeng; Chen, Yongmei; Liu, Bin; Ma, Xiuying; (109 pag.)CN105566324; (2016); A;,
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Electric Literature of 1268810-09-8,Some common heterocyclic compound, 1268810-09-8, name is tert-Butyl (1-ethynylcyclopropyl)carbamate, molecular formula is C10H15NO2, 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.

Copper(I) iodide (205.98 mg, 1.08 mmol), tert-butyl 1 -ethynylcyclopropylcarbamate (3.92 g, 21.6 mmol) and azidotrimethylsilane (3.74 g, 32.5 mmol, 4.31 ml) were added to round bottom flask containing DMF and H20 (50 mL, 9:1). The resulting mixture was stirred under an argon atmosphere at 100 C for 12 h. The mixture was cooled to r.t., diluted with ethyl acetate (200 mL) and filtered through a pad of silica gel. The filtrate was washed with water (3 x 300mL), dried over Na2SO4 and concentrated under reduced pressure to give tert-butyl N-[1-(1H-1 ,2,3-tria.zol-5-yl)cyclopropyl]carbarnate (3.46 g, 15.4 mmol, 71.3% yield) as brown solid.

The synthetic route of 1268810-09-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AICURIS GMBH & CO. KG; DONALD, Alastair; URBAN, Andreas; BONSMANN, Susanne; WEGERT, Anita; GREMMEN, Christiaan; SPRINGER, Jasper; (376 pag.)WO2019/86141; (2019); A1;,
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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;,
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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,
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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;,
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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;,
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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;,
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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;,
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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

Adding a certain compound to certain chemical reactions, such as: 119023-25-5, name is 2-Amino-4-fluorobenzamide, 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 119023-25-5, Formula: C7H7FN2O

Stage 3: 2-aminomethyl-5-fluorophenylamine 2 M borane-dimethyl sulfide complex (40 ml, 80 mmol) in tetrahydrofuran was added to a solution of the product from stage 2 (2.45 g, 16 mmol) in anhydrous tetrahydrofuran (50 ml) and the mixture was heated under reflux for 9 hours. Water (4 ml) was cautiously added to the cooled reaction solution and the mixture was then concentrated in vacuo. Toluene (2*) was added to the residue and the mixture was concentrated again each time. The residue was then repeatedly dissolved in methanol (3*) and concentrated each time. The crude product was purified by flash chromatography with chloroform/methanol (7:3) and 1% triethylamine. Yield: 1.37 g (61%), white solid. Melting point: 49-51 C.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Amino-4-fluorobenzamide, and friends who are interested can also refer to it.

Reference:
Patent; Gruenenthal GmbH; US2008/293749; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics