Category: amides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 134575-14-7, name is exo-Benzyl 6-(hydroxymethyl)-3-azabicyclo[3.1.0]hexane-3-carboxylate, 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 134575-14-7, name: exo-Benzyl 6-(hydroxymethyl)-3-azabicyclo[3.1.0]hexane-3-carboxylate

24.2. (la,5a,6a)-6-Formyl-3-aza-bicyclo[3.1.0]hexane-3-carboxylic acid benzyl ester:DMP (15% in DCM, 20 mL) was added to a solution of intermediate 24.1 (1.27 g) in DCM (20 mL) at RT. After stirring for 2h40 at RT, sat. aq. NaHCO3 was added and the phases were separated. The org. phase was dried (MgSO^ and evaporated off. CC (Hept/EA 12/88 to EA) of the crude afforded 620 mg of the desired compound as orange oil.LC-MS: tR = 0.86 min; [M+H]+: 246.04.

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Reference:
Patent; ACTELION PHARMACEUTICALS LTD; CAROFF, Eva; HILPERT, Kurt; HUBLER, Francis; MEYER, Emmanuel; RENNEBERG, Dorte; WO2010/116328; (2010); A2;,
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Synthetic Route of 19962-04-0, These common heterocyclic compound, 19962-04-0, name is 3-Aminophenyl dimethylcarbamate, 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. Preparation of tert-butyl 4-(tert-butoxycarbonylamino)-4-(3-(dimethylcarbamoyloxy)phenylcarbamoyl)piperidine-1-carboxylate. N-Boc-amino-(4-N-Boc-piperidinyl)carboxylic acid (0.114 g, 0.33 mmol), HATU (0.151 g, 0.40 mmol) and N,N-diisopropylethylamine (128 mg, 1.0 mmol) were combined in isopropyl acetate (2.3 mL) and stirred at room temperature for 15 minutes. 3-aminophenyl dimethylcarbamate (0.072 g, 0.40 mmol) was added, and the mixture heated at 80 C. for 1.5 hours. The reaction mixture was allowed to cool, diluted with EtOAc, washed with 2 N Na2CO3, 1 N HCl, and brine, and then dried over MgSO4 and concentrated. Purification by silica gel chromatography (60% EtOAc/hexanes) gave the title compound (0.075 g, 45%) as a white solid. MS (ES+) [M+NH4]+=524.

The synthetic route of 19962-04-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Burgoon, Hugh Alfred; Goodwin, Nicole Cathleen; Harrison, Bryce Alden; Healy, Jason Patrick; Liu, Ying; Mabon, Ross; Marinelli, Brett; Rawlins, David Brent; Rice, Dennis Stewart; Whitlock, Norris Andrew; US2009/264450; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 621-38-5, 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. 621-38-5, name is 3-Bromoacetanilide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Methyllithium (1.4 M in diethyl ether, 37.4 ml, 52.3 mmol) was added to a -78 C. solution of 3-bromoacetanilide (11.5 g, 53.7 mmol) in tetrahydrofuran (250 ml). The reaction was stirred 15 min at -78 C. Tert-butyllithium (1.7 M in pentane, 62.4 ml, 106 mmol) was added over 30 min to the -78 C. reaction mixture. The reaction was stirred 10 min at -78 C. N-methoxy-N-methyl (1-methyl(4-piperidyl))formamide (5.0 g, 26.8 mmol) in tetrahydrofuran (20 ml) was added dropwise to give a homogeneous yellow solution. The reaction mixture was stirred and allowed to warm to room temperature over 21 hours. The reaction mixture was cooled to 10 C., quenched with ice, and extracted with 1N hydrochloric acid solution. The aqueous extracts were washed with diethyl ether, basified to pH 12 with 5N sodium hydroxide solution and extracted with diethyl ether. The diethyl ether extracts were dried over sodium sulfate and the solvent was removed under reduced pressure to give 6.1 g of a yellow oil. The basic aqueous solution was again extracted with chloroform/isopropanol (3:1). These extracts were dried over sodium sulfate and the solvent was removed under reduced pressure to give 3.4 g of a yellow oil. Both oils were combined and purified by flash chromatography (silica gel, methylene chloride:methanol:ammonium hydroxide, 100:7.5:0.75) to yield 5.7 g (81%) of product as a yellow oil. [00418] MS(m/e): 261(M+1), 259(M-1).

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, 3-Bromoacetanilide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Eli Lilly and Company; US6777428; (2004); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 406233-31-6, 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 406233-31-6 as follows.

Into a1 OO-mL round-bottom flask, was placed 4-fluoro-3-nitrobenzene- 1- sulfonamide (1.43 g, 0.007 mmol, 1 equiv), i-[(25)-i,4-dioxan-2-yljmethanamine hydrochloride (1 g, 6.5 10 mmol, 1 equiv), THF (30 mL), Cs2CO3 (8.48 g, 0.026 mmol, 4 equiv). The resulting solution was stirred overnight at 50C in an oil bath. The solids were collected by filtration. The solid was dried in an oven under reduced pressure. This resulted in 1.82 g (88.10%) of 4-([[(25)-i,4-dioxan-2- ylj methylj amino)-3 -nitrobenzene- 1- sulfonamide as a yellow solid. LC-MS: (ES, m/z):M+i=318, R,T= 0.741 mm. ee=99%, [aj = -17.4 (C= 0.102 g in 100 ml DMSO, T=27C).

According to the analysis of related databases, 406233-31-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NEWAVE PHARMACEUTICAL INC.; CHEN, Yi; LOU, Yan; (108 pag.)WO2019/40550; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 2618-96-4, These common heterocyclic compound, 2618-96-4, name is Dibenzenesulfonimide, 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: Under N2, ynamide 1a (0.300 mmol, 108.7 mg) and diphenylsulfonimide (2a; 0.600 mmol, 178.4 mg, 2.00 equiv) were dissolved in CH2Cl2 (4.00 mL). The reaction mixture was allowed to stir at r.t. After the consumption of 1a (4.5 h, TLC, eluent: PE-EtOAc, 4:1), the mixture was concentrated, and the residue was purified by flash chromatography on silica gel (eluent: PE-EtOAc, 6:1 ? 4:1) to afford 3a.

The synthetic route of 2618-96-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yu, Lian; Deng, Yuan; Cao, Jian; Synthesis; vol. 47; 6; (2015); p. 783 – 788;,
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. 2297-06-5, name is Methyl 4-amino-2-sulfamoylbenzoate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H10N2O4S

SYNTHESIS EXAMPLE 5 Synthesis of preparation intermediate, methyl 2-(aminosulfonyl)-4-(2,5-dihydro-3,4-dimethyl-2,5-dioxo-1H-pyrrol-1-yl)benzoate (Compound No. II-B-4) In 3 ml of acetic acid, 1 mmol of methyl 4-amino-2-(aminosulfonyl)benzoate and 1.05 mmol of 2,3-dimethylmaleic anhydride were stirred at 80 C. for 40 hours. Acetic acid was then distilled off from the reaction mixture, followed by the addition of 20 ml of ice water to the oily residue. After the mixture thus formed was stirred for 2 hours, the resulting precipitate was collected by filtration and then dried in air. Yield: 43%. Its physiocochemical properties are shown in Table 8.

The synthetic route of 2297-06-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kureha Kagaku Kogyo K.K.; US5127937; (1992); A;,
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

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