Category: 456-64-4

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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., category: amides-buliding-blocks

6-Oxo-6,7-dihydro-thieno[2,3-b]pyridine-5-carboxylic acid methyl ester described in Preparation Example T-8 (9mg, 43mumol), N-phenyltrifluoromethanesulfonimide (23mg, 65mumol) and dimethyl-pyridin-4-yl-amine (catalytic amount) were dissolved in dichloromethane (0.5mL), and the solution was stirred for 18.5 hours at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate, the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, the residue was purified by NH silica gel column chromatography (hexane : ethyl acetate = 3 : 1), and the title compound (10mg, 29mumol, 68%) was obtained as a white solid. 1H-NMR Spectrum (CDCl3) delta(ppm) : 4.03 (3H, s), 7.43 (1H, d, J=5.9Hz), 7.73 (1H, d, J=5.9Hz), 8.87 (1H, s).

According to the analysis of related databases, 456-64-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Eisai Co., Ltd.; EP1669348; (2006); 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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., Quality Control of 1,1,1-Trifluoro-N-phenylmethanesulfonamide

Step E-Methyl 3-({(1R)-1-[2-(trifluoromethyl)phenyl]ethyl}oxy)-5-(6-{[(trifluoromethyl)sulfonyl]oxy}-1H-benzimidazol-1-yl)-2-thiophenecarboxylate To a stirred, cooled (0 C.) solution of methyl 5-(6-hydroxy-1H-benzimidazol-1-yl)-3-({(1R)-1-[2-(trifluoromethyl)phenyl]ethyl}oxy)-2-thiophenecarboxylate (2.49 g, 5.38 mmol) and n-phenyltrifluoromethane sulfonamide (2.06 g, 5.76 mmol) in DCM (30 mL) was added diisopropylethylamine (2.0 mL, 11.5 mmol). The reaction was allowed to warm to room temperature and stirred for 12 h. The reaction mixture was then concentrated under vacuum, and chromatographed on silica gel (120 g), eluding with a 5-to-40% gradient of EtOAc/hexane to give 3.12 g (98%) of the title compound as a light yellow solid. 1H NMR (400 MHz, DMSO-d6): delta 8.76 (s, 1H), 8.01-7.94 (m, 2H), 7.80-7.70 (m, 3H), 7.56-7.43 (m, 3H), 5.98 (q, 1H, J=6.10 Hz), 3.84 (s, 3H), 1.65 (d, 3H, J=6.22 Hz); MS (ESI): 595 [M+H]+.

The synthetic route of 456-64-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dar, Mohammed; US2009/5398; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,1,1-Trifluoro-N-phenylmethanesulfonamide

tert-Butyl 4-{ [(trifluoromethyl)sulfonyl] oxy}-3,6-dihydropyridine-l(2H)-carboxylateDi-wo-propylamine (22 ml) was dissolved in dry THF (125 ml) and cooled to -78C. «-Butyllithium (62.5 ml, 2.5M) was added dropwise. The solution was stirred for 15 minutes, then tert-bntyl 4-oxopiperidine-l-carboxylate (28.32 g) in THF (100 ml) was added dropwise. The reaction mixture was stirred for 1 hour at -78C, then N- phenyltrifluoromethanesulfonimide (53.8 g) in THF (150 ml) was added dropwise. The reaction mixture was stirred at -78C for 2 hours and allowed to warm up to room temperature and stirred overnight. The reaction mixture was then concentrated in vacuo and the residue dissolved in ether (1000 ml). This was washed with water (500 ml), 2M sodium hydroxide solution (3 x 500 ml), water (500 ml) and brine (500 ml) then dried over magnesium sulfate and concentrated to give the title compound as a pale brown oil (45.38 g, 96%) which was used without further purification; 1H NMR (CDCl3) deltal.48 (9H, s), 2.44 (2H, m), 3.63 (2H, t), 4.00 (2H, q), 5.70 (IH, br m).

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 456-64-4.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2007/60408; (2007); A2;,
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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., Recommanded Product: 456-64-4

Compound 60; N-phenytrifluoromethanesulfonimide (3.336 g, 9.337 mmol, 1.1 eq.) was added to Compound 53 (2.37 g, 8.488 inmol, 1.0 eq.) in 100 mL DCM, followed by Cs2CO3 (3.04 g, 1.1 eq.). The reaction mixture was stirred at room temperature for 12 hours. The reaction mixture was filtered through CELITE and concentrated. The residue was purified by silica gel chromatography (30-60% EtOAc/hexane) to give Compound 60 as the white solid (3.2 g, 92%). 1H NMR (300 MHz, CDCl3): delta 7.37 (d, 2 H), 7.20 (d, 2 H), 4.50 (m, 1 H), 4.18 (m, 1 H), 3.03 (m, 1 H), 2.98 (m, 2 H), 2.85 (m, 1 H), 2.62 (m, 1 H), 1.39 (s, 9 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; GILEAD SCIENCES, INC.; WO2008/11117; (2008); A2;,
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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., Product Details of 456-64-4

Example 4 Preparation of; A solution of N-phenyltrifluoromethanesulfonamide (0.97 g) and N,N-diisopropylethylamine (0.58 g) in dry THF (3.9 g) was added to a stirred solution of the product of Preparative Example 3 (1.0 g) in dry THF (4.0 g) within a round bottom flask. This mixture was allowed to stir overnight. The volatile components were then removed using a rotary evaporator. The residue was dissolved in chloroform (40 mL) and was washed first with 0.1N aqueous HCl (40 mL) and then with saturated aqueous sodium chloride. The organic phase was dried over magnesium sulfate and was then filtered. The volatile components were removed using a rotary evaporator to afford 1.03 g of product.

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; 3M Innovative Properties Company; US2005/107615; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., category: amides-buliding-blocks

6-Oxo-6,7-dihydro-thieno[2,3-b]pyridine-5-carboxylic acid methyl ester described in Preparation Example T-8 (9mg, 43mumol), N-phenyltrifluoromethanesulfonimide (23mg, 65mumol) and dimethyl-pyridin-4-yl-amine (catalytic amount) were dissolved in dichloromethane (0.5mL), and the solution was stirred for 18.5 hours at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate, the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, the residue was purified by NH silica gel column chromatography (hexane : ethyl acetate = 3 : 1), and the title compound (10mg, 29mumol, 68%) was obtained as a white solid. 1H-NMR Spectrum (CDCl3) delta(ppm) : 4.03 (3H, s), 7.43 (1H, d, J=5.9Hz), 7.73 (1H, d, J=5.9Hz), 8.87 (1H, s).

According to the analysis of related databases, 456-64-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Eisai Co., Ltd.; EP1669348; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 456-64-4, 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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a-78 C solution of Preparation 30 (7.0 g, 19.1 mmol) in THF (80 mL) add potassium hexamethyldisilane (KHMDS) (53 mL, 0.5 M solution in toluene, 26.7 mmol) over 5 min. Add hexamethylphosphoramide (HMPA) (4.64 mL, 26.7 mmol) quickly, and stir the solution at-78 C for 25 min. Add a solution of N-phenyl triflamide (11.5 g, 32.2 mmol) in THF (15 mL + rinse) via syringe. Maintain the resulting solution at-78 C for 2 h, then pour the reaction contents into 1/2 SATD. NAHCO3 AND extract with ET20 (150 ML) and EtOAc (2 x 75 mL). Wash the combined organic extracts with H2O (2 x 100 mL) and brine (100 mL), dry over NA2SO4, and concentrate. Purification of the crude product by MPLC (0 to 12 to 25% EtOAc/hexanes) affords Preparation 31 (6.25 g, 66%) as an OFF-WHITE SOLID. H NMR (CDC13) 8 7.25-7. 43 (m, 5 H), 6. 84 (d, J = 8.8 Hz, 1 H), 6. 80 (dd, J = 8.8, 2.8 Hz, 1 H), 6.72 (d, J = 2. 8 Hz, 1 H), 5.02 (s, 2 H), 4.04 (m, 4 H), 3. 82 (dd, J = 4.4, 12. 8 Hz, 1 H), 2.66 (dq, J = 14.0, 2.4 Hz, 1 H), 2.21 (m, 2 H), 1.91 (m, 1 H), 1. 80 (t, J = 12.8 Hz, 1 H), 1.64 (TD, J = 12.8, 4.4 Hz, 1 H).

The synthetic route of 1,1,1-Trifluoro-N-phenylmethanesulfonamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2004/94400; (2004); A2;,
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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., SDS of cas: 456-64-4

The free phenolic hydroxy was then triflated to give 39.; Compound 39; To a solution of 38 (324 mg, 1.50 mmol) in CH2C12 (20 mL) at RT, PhNHTf (639 mg, 1.8 0 mmol) was added at once. NEt3 (417 uL, 3.0 mmol) was added dropwise over 5 min. The reaction mixture was stirred at RT for 10 hr. The solvents were removed in vacuo. The residue was purified by silica gel flash chromatography with 6:1 Hex/EtOAc to give the title compound (454 mg, 87%) . XH NMR (400 MHz, CDCI3) : 8, 2.68 (s, 3H) , 3.89 (m, 2H) , 4.70 (d, J = 17.4 Hz, 1H) , 5.20 (d, J = 10.4 Hz, 1H) , 6.03 (m, 1H) , 6.34 (s, 1H) , 7.36 (d, J= 9.2 Hz, 2H) , 7.47 (d, J = 9.2 Hz, 2H) . 13C NMR (100 MHz, CDCI3) : 8, 24.1, 31.3, 117.4, 117.9, 118.8, 120.7, 124.1, 130.8, 134.4, 144.6, 152.3,153.5, 158.8. IR umax(NaCl)/cm-1: 1727, 1428,1216, 1135, 965. MS (APCI+) calculated for C14H11F3O5S ml z 348.30, observed mlz 348.8.

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; THE TRUSTEES OF COLLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; WO2006/26368; (2006); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, 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 456-64-4, Formula: C7H6F3NO2S

EXAMPLE 50 3-Methyl-2-[5-(trifluoromethanesulfonamido)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene To a solution of 500 mg (1.82 mmol) of 3-methyl-2-[5-(amino)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene in 30 ml of acetonitrile were added 0.51 ml (3.66 mmol) of triethylamine and 1.302 g (3.66 mmol) of N-phenyltrifluoromethanesulfonamide. The mixture was stirred for two hours at room temperature. The solvent was distilled off. To the residue was added methylene chloride, which was washed with water, and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: ethyl acetate) to afford 608 mg (82.1%, a pale yellow solid) of the desired compound. NMR(200 MHz,CDCl3)delta: 1.55-1.85(4H,m), 1.97(2H,m), 2.90(3H,s), 3.39(2H,m), 3.50(2H,t,J=7.0 Hz), 7.69(1H,d,J=7.8 Hz), 7.73(1H,d,J=8.0 Hz), 7.95(1H,dd,J=8.0, 7.8 Hz).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,1-Trifluoro-N-phenylmethanesulfonamide, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US5958942; (1999); 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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., Safety of 1,1,1-Trifluoro-N-phenylmethanesulfonamide

To a solution of N-carbethoxy-4-tropinone (2-1) (15.0 g, 76.1 mmol) in 150 mL anhydrous tetrahydrofuran at-78 C was slowly added KN (TMS) 2 (182 mL, 0.5 ML in toluene). The solution was stirred at-78 C for 30 minutes, and then a solution of N-phenyltrifluoromethane sulfonamide (32.6 g, 91. 3 mmol) in 150 mL anhydrous tetrahydrofuran was added. The mixture was stirred at-78 C for 2 h and quenched with a saturated aqueous ammonium chloride (150 mL). After the removal of tetrahydrofuran under vacuum, the aqueous layer was then extracted with EtOAc (3 x 150 mL). The combined EtOAc layers were washed with IN KOH (150 ml), brine, dried over anhydrous magnesium sulfate, filtered, and concentrated. Purification of the crude residue by flash chromatography over silica gel (gradient elution; 0%-30% ethyl acetate/hexanes as eluent) afforded (2-2) as a colorless oil.

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; MERCK & CO., INC.; WO2004/87159; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics