2-methyl-N-(oxomethylidene)benzenesulfonamide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 16.1 g of polypropylene glycol (M=480), 65.7 g of anhydrous tetrahydrofuran and 0.22 g of toluenesulfonyl isocyanate were stirred for 15 minutes in a three-necked flask with a capacity of 250 ml. 13 g of tolylene-2,4-diisocyanate and 0.17 g of dibutyltin dilaurate were then added and the mixture was heated under reflux for two hours. 6.9 g of the addition product formed from 1 mol of succinic anhydride and 1 mol of diethanolamine were then added and refluxing was continued for a further two hours. The solution was then diluted with 42.2 g of tetrahydrofuran and 1.95 g of polyoxypropylenediamine (M=420) in 42.2 g of tetrahydrofuran were added dropwise. the mixture was heated under reflux for two hours

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 17.8 g of polypropylene glycol (M=480), 0.24 g of toluenesulfonyl isocyanate and 150 g of anhydrous tetrahydrofuran were stirred for 15 minutes in a three-necked flask with a capacity of 250 ml. 13.0 g of tolylene 2,4-diisocyanate and 0.17 g of dibutyltin dilaurate were then added, the mixture was refluxed for one hour, and the solution obtained was added dropwise to a mixture of 7.6 g of the monoamide formed from 1 mol of succinic anhydride and 1 mol of diethanolamine in 184 g of tetrahydrofuran and heated for 22 hours under reflux until isocyanate was no longer present in the solution. A weight average of the molecular weight (Mw) of 8500 was determined with the aid of gel permeation chromatography (polystyrene standard). the mixture was refluxed for one hour the solution obtained was added dropwise to a mixture of 7.6 g of the monoamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 16.1 g of polypropylene glycol (M=480), 65.7 g of anhydrous tetrahydrofuran and 0.22 g of toluenesulfonyl isocyanate were stirred for 15 minutes in a three-necked flask with a capacity of 250 ml. 13 g of tolylene-2,4-diisocyanate and 0.17 g of dibutyltin dilaurate were then added and the mixture was heated under reflux for two hours. 6.9 g of the addition product formed from 1 mol of succinic anhydride and 1 mol of diethanolamine were then added and refluxing was continued for a further two hours. The solution was then diluted with 42.2 g of tetrahydrofuran and 1.95 g of polyoxypropylenediamine (M=420) in 42.2 g of tetrahydrofuran were added dropwise. the mixture was heated under reflux for two hours

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 17.8 g of polypropylene glycol (M=480), 0.24 g of toluenesulfonyl isocyanate and 150 g of anhydrous tetrahydrofuran were stirred for 15 minutes in a three-necked flask with a capacity of 250 ml. 13.0 g of tolylene 2,4-diisocyanate and 0.17 g of dibutyltin dilaurate were then added, the mixture was refluxed for one hour, and the solution obtained was added dropwise to a mixture of 7.6 g of the monoamide formed from 1 mol of succinic anhydride and 1 mol of diethanolamine in 184 g of tetrahydrofuran and heated for 22 hours under reflux until isocyanate was no longer present in the solution. A weight average of the molecular weight (Mw) of 8500 was determined with the aid of gel permeation chromatography (polystyrene standard). the mixture was refluxed for one hour the solution obtained was added dropwise to a mixture of 7.6 g of the monoamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred solution of 0.85 g of 2-amino-4-dimethylamino-6-methoxy-1,3,5-triazine in 40 ml of methylene chloride was added, dropwise, 1.0 g of 2-methylbenzenesulfonyl isocyanate in 10 ml of methylene chloride. After stirring 24 hours, the resulting solution was evaporated to yield a solid. Recrystallization from benzene/hexane yielded the product named above melting at 194°-198°. the resulting solution was evaporated to yield a solid Recrystallization from benzene/hexane yielded the product

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a stirred mixture of 2.40 g of 4-amino-2,6-dimethoxypyrimidine in 40 ml methylene chloride at ambient temperature and pressure was slowly added 3.0 g of 2-methylbenzenesulfonylisocyanate. The reaction was stirred 40 minutes, filtered, and the solid thereby obtained was washed with a small amount of acetonitrile; yield 4.0 g, m.p. 174°-175°, NMR (DMSO-d6) relative to tetramethylsilane: δ 2.77, S, area 30; δ 4.05, S, area 60; δ 6.85, S, area 89; δ 7.7-8.6, multiplets, area 45; δ 10.00, S, area 9. filtered the solid thereby obtained was washed with a small amount of acetonitrile

反応条件: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-(4-chloro-2-hydroxymethyl-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.050 g, 0.12 mmol) in dry toluene (2 mL) was added triethylamine (0.05 mL, 0.36 mmol) followed by o-toluenesulfonylisocyanate (0.05 mL, 0.36 mmol) and catalytic 4-dimethylaminopyridine. After 23 hours the reaction was warmed to 55° C. for 2 hours. After cooling the reaction was evaporated to dryness and the title compound purified by silica gel chromatography (0.074 g, LRMS: 618.1). After cooling the reaction was evaporated to dryness the title compound purified by silica gel chromatography (0.074 g, LRMS: 618.1)

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A three-necked flask equipped with a dropping funnel, a thermometer, and a reflux condenser was charged with 18.6 g of aniline and the aniline was dissolved in 200 ml of toluene. While the resultant reaction solution was stirred with a magnetic stirrer, 42.0 g of toluenesulfonylisocyanate were added dropwise from the dropping funnel to the reaction solution. During the stirring, an exothermic reaction occurred and a large amount of white solid was precipitated. The resultant reaction mixture was heated at a temperature of 90° C. for one hour, cooled, and then filtered. White crystals were obtained in an amount of 58.0 g. The crystals had a melting point of 166° C. A three-necked flask equipped with a dropping funnel While the resultant reaction solution During the stirring, an exothermic reaction a large amount of white solid was precipitated The resultant reaction mixture cooled filtered White crystals were obtained in an amount of 58.0 g