Month: January 2021

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. 103-89-9, name is 4′-Methylacetanilide, A new synthetic method of this compound is introduced below., Recommanded Product: 4′-Methylacetanilide

1a as example: To a stirred suspension of N-(p-tolyl)acetamide 1a (75 mg, 0.5 mmol) and Selectfluor (213 mg, 0.6 mmol) in water (3.0 mL) was added HBr (40% aqueous, 0.08 mL, 0.55 mmol), and the mixture was stirred for 5 min at room temperature. After 1a was consumed, as indicated by TLC, the reaction mixture was quenched with saturated aqueous Na2S2O3 (2.0 mL) and water (20.0 mL), and extracted with CH2Cl2 (10.0 mL) three times. The residue obtained after evaporation of the solvent was purified by column chromatography on silica gel (petroleum ether-ethyl acetate = 6:1, v/v) to afford N-(2-bromo-4-methylphenyl)acetamide 2a as a white solid (108 mg, 95% yield).

The synthetic route of 103-89-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liang, Deqiang; Li, Xiangguang; Wang, Chaowu; Dong, Qishan; Wang, Baoling; Wang, Hai; Tetrahedron Letters; vol. 57; 48; (2016); p. 5390 – 5394;,
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Application of 3984-14-3, 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. 3984-14-3, name is N,N-Dimethylsulfamide, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of ethyl 4-{[3-chloro-4-(trifluoromethyl)phenoxy]methyl}benzoate (Preparation 18, 125 mg, 0.35 mmol) in methanol (5.0 ml) was added water (2.0 ml_) followed by sodium hydroxide (140 mg, 3.5 mmol). The reaction mixture was heated to 55C for 18 hours, then cooled and diluted with EtOAc (50 ml_) and 2M HCI (50 ml_). The aqueous layer was separated and washed with EtOAc (2 x 50 ml_). The combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo to yield 4-{[3-chloro-4-(trifluoromethyl)phenoxy]methyl}benzoic acid as an off-white solid (90 mg, 78% yield). This solid was dissolved in dichloromethane (3ml_) then EDCI (344 mg, 1 .79 mmol) and DMAP (88 mg, 0.70 mmol) were added, followed by the addition of N,N- dimethylsulfamide (86 mg, 0.70 mmol). The reaction was left to stir at room temperature for 2 hours. A solution of 2M HCI (10ml) was added and the mixture separated using a phase separation cartridge. The organics were dried in vacuo to yield a solid which was triturated with heptane:IPA (4:1 , 100 mL) and sonicated. The supernatant was decanted and the residue dried in vacuo to yield an off-white solid as the title compound (57 mg, 38% yield). 1 H NMR (400 MHz, CDCI3): delta 3.05 (s, 6H), 5.17 (s, 2H), 6.90 (m, 1 H), 7.10 (d, 1 H), 7.54 (d, 2H), 7.61 (d, 1 H), 7.86 (d, 2H), 8.51 (br s,1 H). LCMS Rt = 1 .56 minutes MS m/z 435 [M35CI-H]-

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

Reference:
Patent; PFIZER LIMITED; RAWSON, David James; STORER, Robert Ian; SWAIN, Nigel Alan; WO2013/88315; (2013); A1;,
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2675-89-0, name is 2-Chloro-N,N-dimethylacetamide, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C4H8ClNO

A mixture of (S)-2-({2-[3-(lH-Indazol-4-yl)-propylamino]-4,6-dimethyl-pyrimidine-5- carbonyl}-amino)-3-[(thiophene-2-carbonyl)-amino]-propionic acid (0.05g, 0.095mmol), 2- chlorodimethyl acetamide (0.017g, 0.143mmol), sodium iodide (0.021g, 0.143mmol), and potassium carbonate (0.020g, 0.143mmol) in DMF (1ml) was stirred at rt overnight. The mixture was diluted with EtOAc, washed with brine, dried over Na2S04, filtered, concentrated the presence of silica gel and chromatographed (100% EtOAc) to give the desired product (38.8mg, 67% yield). MS m/e 607.1 (M+H+).

The synthetic route of 2675-89-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GILLESPIE, Paul; MICHOUD, Christophe; RUPERT, Kenneth Carey; THAKKAR, Kshitij Chhabilbhai; YI, Lin; WO2012/123467; (2012); A1;,
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202207-79-2, name is 1-(Boc-amino)-2-(methylamino)ethane Hydrochloride, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: 1-(Boc-amino)-2-(methylamino)ethane Hydrochloride

A solution of tert-butyl [2-(methylamino)ethyl]carbamate hydrochloride (0.30 g, 0.0014 mol), 2-chloropyridine (160 mg, 0.0014 mol), and triethylamine (300 muL, 0.0021 mol) in acetonitrile (5 mL) was heated at 90 C. overnight. The mixture was diluted with methanol, and purified by RP-HPLC (pH=10) to afford the desired product. Analytical LCMS: (M+H)+=252.1

The synthetic route of 202207-79-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INCYTE CORPORATION; US2008/39457; (2008); A1;,
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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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,1,1-Trifluoro-N-phenylmethanesulfonamide

A solution of 6-piperidin-1-ylmethyl-pyridin-3-ol (0.225 g, 1.17 mmol), N-phenyltriflouromethanesulfonamide (0.50 g, 1.41 mmol), and TEA (0.50 mL, 3.50 mmol) in DCM (20 mL) was heated at reflux for 18 h. The solvent was removed and chromatography of the residue (SiO2: 0-3% 2 M NH3 in MeOH/DCM) gave the title compound as a solid (0.036 g, 95%).

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; Carruthers, Nicholas I.; Shah, Chandravadan R.; Swanson, Devin M.; US2005/222151; (2005); A1;,
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192436-83-2, name is 4-Bromo-N-methoxy-N-methylbenzamide, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C9H10BrNO2

To a stirred solution of 2-fluoro-4-bromoanisole (3.03 g, 14.8 mmol) in anhydrous THF (100 mL) was added n-butyllithium (1.6 M in hexanes, 10.2 mL, 16.3 mol) dropwise at-78 C. The reaction mixture was stirred for 1 h and 80 (4.02 g, 16.3 mmol) dissolved in THF (20 mL) was added dropwise. The reaction mixture was warmed to-20 C over 1 h, water (100 mL) was added, and the volatiles were removed under reduced pressure. The mixture was extracted with ether (3 x 100 mL) and the combined extracts were washed with water (100 mL) and brine (100 mL). The mixture was dried over MgS04 and concentrated. The residue was chromatographed on silica gel (20: 1 to 5: 1 hexanes: EtOAc) to afford 2.35 g (51%) of 81 as a white crystalline SOLID. H NMR (400 MHz, CDCI3) : 8 3.97 (s, 3H), 7.01 (t, J = 8.4 Hz, 1 H), 7.55-7. 62 (m, 6H).

The synthetic route of 192436-83-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2005/12220; (2005); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide, 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 830-43-3, SDS of cas: 830-43-3

Step b N-[(1-Oxo-2-oxo-2-chloro)ethyl]-4-(trifluoromethyl)benzenesulfonamide Combine 4-(trifluoromethyl)benzenesulfonamide (1.44g, 6.4mmol) and oxalyl chloride (15mL) and reflux for 9 hours. Evaporate the excess oxalyl chloride in vacuo to give the title compound.

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, 4-(Trifluoromethyl)benzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Merrell Pharmaceuticals Inc.; US5606063; (1997); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 533-17-5, name is N-(2-chlorophenyl)acetamide, 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 533-17-5, Formula: C8H8ClNO

General procedure: A mixture of N-phenylacetamide(2a, 135 mg, 1.0 mmol), iodine (254 mg, 1 mmol), TBHP (387 mg, 3.0 mmol, 70% in water) and toluene (2.0 mL) was added successively in a round-bottom flask, and the resulting soln. stirred for 24 h at 80 C. The mixture was then subjected to purification by preparative thin-layer chromatography (PE-EtOAc, 10:3) to afford product 3aa.

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

Reference:
Conference Paper; Chen, Cui; Liu, Weibing; Zhou, Peng; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 2250 – 2255;,
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Electric Literature of 518057-72-2, 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 518057-72-2 as follows.

To 5-amino-2-fluoro-benzamide (37 mg, 0.24 mmol) and diisopropylethylamine (124 mu, 0.71 mmol) in dichloromethane (390 mu) cooled at 0 C was added dropwise a solution of 2-fluoro-6-(4- fluorophenoxy)-3-(trifluoromethyl)benzoyl chloride (80 mg, 0.24 mmol) in dichloromethane (390 mu). The reaction was stirred at room temperature for 1 hour. The solvent was evaporated and the residue was partitioned between water and ethyl acetate. The organic phase was concentrated to dryness. The residue was dissolved in 1ml of DMSO and purified by reverse phase HPLC to afford N-(3 -carbamoyl -4-fluoro- phenyl)-2-fluoro-6-(4-fluorophenoxy)-3-(trifluoromethyl)benzamide (25.5 mg, 24%). ESI-MS m/z calc. 454.08, found 455.1 (M+l)+; retention time (Method B): 1.63 minutes (3 minute run). l NMR (400 MHz, DMSO-d6) delta 11.05 (s, 1H), 7.98 (dd, J = 6.4, 2.8 Hz, 1H), 7.89 – 7.74 (m, 3H), 7.71 (s, 1H), 7.40 – 7.25 (m, 5H), 6.79 (d, J = 8.9 Hz, 1H) ppm.

According to the analysis of related databases, 518057-72-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; AHMAD, Nadia; ANDERSON, Corey; ARUMUGAM, Vijayalaksmi; ASGIAN, Iuliana, Luci; CAMP, Joanne, Louise; FANNING, Lev Tyler, Dewey; HADIDA RUAH, Sara, Sabina; HURLEY, Dennis; SCHMIDT, Yvonne; SHAW, David; SHETH, Urvi, Jagdishbhai; THOMSON, Stephen, Andrew; (691 pag.)WO2019/14352; (2019); A1;,
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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. 1118-69-0, name is N-Isopropylacetamide, A new synthetic method of this compound is introduced below., Safety of N-Isopropylacetamide

Under nitrogen atmosphere, add 1 -(4-amidogen-2, 6-difluoro-phenyl)-3-N,N-dimethylammonium-2-fluoro-2-acrylketone (IV) (2.5 g, 10 mmol), N-isopropyl acetamide (2.0 g, 20 mmol), phosphorus trichloride (2.0 g, 13 mmol) and methylbenzene 50 mE, 0-5 C., and add triethylamine (2.0 g, 20 mmol) while stirring, and then, raise the temperature to 105-115 C. and conduct stirring operations for 3-5 hours. Reduce the pressure and recycle the solvent, and dissolve the leftovers with dichlormethane 100 mE, and wash with saturated sodium bicarbonate and water, and use anhydrous sodium sulfate for drying and concentration, and obtain yellow solid N-[2,6-difluoro-4-(3-N,N-dimethylam- monium-2-fluoro-2-acrylketone- 1 -yl)phenyl] -N?-isopropylethanamidine (V) 2.8 g, the yield rate is 85.6%; mass spectrum (El): mlz 328 (M+H).

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; SUZHOU MIRACPHARMA TECHNOLOGY CO., LTD.; Xu, Xuenong; (9 pag.)US2017/305884; (2017); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics