Tag: M.W=0-100

Adding some certain compound to certain chemical reactions, such as: 7341-96-0, name is Propiolamide, 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 7341-96-0. 7341-96-0

The imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and inter-methoxyphenyl diazo acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is formula (c) is shown. The yield is 90%, dr value is equal to the 95:5. The product of the1As shown in Figure 5, H NMR schematic view thereof13C NMR schematic view as shown in Figure 6.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of Propiolamide.

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
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. 7803-58-9, name is Sulfuric diamide, A new synthetic method of this compound is introduced below., 7803-58-9

The preparation of sulfamide 16.1 is starting with commercially available, literature or readily available diamine. The treatment of diamine 16.1 with sulfamine a under refluxing pyridine affords sulfamine 16.3, which is followed by alkylation of [A-HALO] alkyl ester to give compound 16.4. Basic hydrolysis (LiOH, [H20/THF/MEOH)] of ester gives acid 16.1 as the intermediateds for example 61.

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; SUNESIS PHARMACEUTICALS, INC.; WO2003/106405; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

625-51-4, A common compound: 625-51-4, name is N-(Hydroxymethyl)acetamide, belongs to amides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

EXAMPLE 5 40.8 g (0.4 mol) of acetic anhydride were cooled to 10 C. After this, 16.4 g (0.2 mol) of phosphorous acid were introduced in the course of 5 minutes, with stirring and cooling. 17.8 g (0.2 mol) of N-hydroxymethylacetamide were subsequently added dropwise at 10 C. in the course of 10 minutes. After this, the mixture was first allowed to come to room temperature and then refluxed for 2.5 hours. The mixture was subsequently cooled. 10 ml of water were then added in portions. After this, the mixture was kept under reflux for 1 hour. After this, a mixture of 10 ml of acetic acid and 1.5 ml of water was added, and stirring was continued. After crystallisation and filtration with suction, 16.3 g (53% of theory) of acetylaminomethanephosphonic acid of a melting point of 188-194 C. were obtained.

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-(Hydroxymethyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoechst Aktiengesellschaft; US5432291; (1995); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 631-58-3, name is Propanethioamide, molecular formula is C3H7NS, 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. 631-58-3

Reference Example H 11 2-ethyl-5-(2-fluoro-4-pyridyl)-4-(3-methylphenyl)-1,3-thiazole A solution of 2-bromo-2-(2-fluoro-4-pyridyl)-1-(3-methylphenyl)ethanone hydrobromide (11 g, 29 mmol) and thiopropionamide (2.7 g, 30 mmol) in N,N-dimethylformamide (30 mL) was stirred for 14 hours at room temperature. Aqueous sodium hydrogen carbonate solution was added to the reaction mixture, and extracted with ethyl acetate. The extracts were washed with water, dried, then, the solvent was distilled off. The residue was purified by silica gel column chromatography (hexane-ethyl acetate= 4:1) to obtain the title compound (3.3 g, yield 38%). oil 1H-NMR (CDCl3) delta: 1.64 (3H, t, J= 7.6 Hz), 2.34 (3H, s), 3.10 (2H, q, J= 7.6 Hz), 6.84-6.86 (1H, m), 7.05-7.09 (1H, m), 7.13-7.25 (3H, m), 7.37 (1H, s), 8.10 (1H, d, J= 5.6 Hz).

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

Reference:
Patent; Takeda Chemical Industries, Ltd.; EP1402900; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

7341-96-0, The chemical industry reduces the impact on the environment during synthesis 7341-96-0, name is Propiolamide, I believe this compound will play a more active role in future production and life.

N-Chlorosuccinimide (624 mg, 4.7 mmol) was added in portions to a solution of 4- bromomethyl-benzaldehyde oxime (which may be prepared as described in Charrier, J.-D. et al. WO2011/143426 p 77; 1 g, 4.7 mmol) in DMF (9 mL) at room temperature. The reaction mixture was stirred for 2 h under argon. The mixture was poured into ice-water and this was extracted with Et2O (3 x 50 mL). The combined organic layers were washed with brine, dried (Na2SO4) and evaporated to give a solid (1.4 g). The solid was dissolved in 50% aqueous tert-butanol (20 mL) in a flask that was open to the air. Propiolamide (which may be prepared as described in Matsumoto, T. et al. US 7,851,473 Column 128; 323 mg, 4.7 mmol) was added, followed by 1 M sodium ascorbate (0.47 mL, 0.47 mmol) and 0.1 M copper(II) sulfate (2.34 mL, 0.23 mmol). KHCO3 (1.87 g, 18.7 mmol) was added in portions and the reaction mixture was stirred at room temperature for 3 h. H2O (25 mL) was added and the mixture was extracted with 85: 15 CHCl3/CH3OH (3 x 100 mL). The combined organic layers were washed with brine, dried (Na2S04), filtered, evaporated, and purified by chromatography (16-20% acetone/CH2Cl2) to give 3-(4-bromomethyl- phenyl)-isoxazole-5-carboxylic acid amide (156 mg, 12%). Purification of mixed fractions by chromatography (16-20% acetone/CH2Cl2) provided a further 40 mg (3%) of 3-(4- bromomethyl-phenyl)-isoxazole-5-carboxylic acid amide.

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

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; ERICKSON, Shawn, David; GILLESPIE, Paul; MERTZ, Eric; WO2014/86704; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 6228-73-5, name is Cyclopropanecarboxamide, 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. 6228-73-5

To a microwave tube was added 4-(4-bromo-lH-imidazo[4,5-c]pyridin-2-yl)-3,5- dichlorobenzonitrile (0.10 g, 0.27 mmol), cyclopropanecarboxamide (0.069 g, 0.81 mmol), Pd2(dba)3 (0.036 g, 0.040 mmol), XantPhos (0.017 g, 0.030 mmol), Cs2C03 (0.26 g, 0.81 mmol) and dioxane (3.0 mL). The mixture was degassed with N2 for 10 min. The resulting mixture was irradiated in a microwave reactor at 160 C for 2 hours and then cooled to room temperature. The mixture was filtered with Celite and the filtrate was concentrated and purified by prep-TLC to give the desired product as a white solid (15 mg, 15 % yield). ? NMR (MeOR-d4, 500 MHz): delta 7.95 (s, 2H), 7.54 (m, 1H), 7.45 (m, 1H), 1.90 (m, 1H), 1.23 – 1.18 (m, 2H), 1.00 – 0.88 (m, 2H). LCMS(ESI) m/z: 372.0 [M+H+].

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 6228-73-5.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; LAI, Yingjie; LIANG, Jun; MAGNUSON, Steven R.; TSUI, Vickie H.; ZHANG, Birong; ROBARGE, Kirk; WO2011/113802; (2011); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics