2-methylsulfonylethanesulfonyl chloride

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-(methylsulfonyl)ethanesulfonyl chloride in 50 ml chloroform, 15.5 g (0.2 mole) 40% methylamine in water were added slowly. The reaction mixture was stirred one hour and then filtered. The filtrate was washed with water. The organic phase was separated and then stripped. Cold ether was added to the residue; the resulting mixture was stirred. Filtration of the ether mixture gave 11.0 g of the above-identified product as a white solid, mp. 116°-117° C. were added slowly filtered The filtrate was washed with water The organic phase was separated Cold ether was added to the residue the resulting mixture was stirred Filtration of the ether mixture

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 5.00 g (24.2 mmoles) 2-(methylsulfonyl)ethylsulfonyl chloride (Example 32) in 50 ml dry tetrahydrofuran, a solution of 2.11 g (0.025 moles) 2-amino-2-methyl-propionitrile and 2.5 g (0.025 moles) triethylamine in 20 ml dry tetrahydrofuran were added dropwise over 13 minutes. During the course of the addition, the temperature of the mixture rose from 19° C. to 38° C. and a white precipitate formed. After the mixture cooled to room temperature, it was filtered. The solid, inorganic salts, was washed with tetrahydrofuran and ethyl ether. The filtrate and washings were stripped using a rotovap to give 8.2 g of a sticky white solid. Recrystallization of the solid from boiling ethanol gave 3.94 g of the above-identified product, melting point 151°-153° C. During the course of the addition rose from 19° C. to 38° C. a white precipitate formed it was filtered The solid, inorganic salts, was washed with tetrahydrofuran and ethyl ether