HRID72347

反应详情

EQUATION

反应方程式

HRID 72347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-(tert-butyl)-2-(4-fluorophenyl)-2-oxoethanesulfonamide (657 mg), ammonium acetate (1.85 g) and sodium cyanoborohydride (166 mg) was stirred in methanol (12 ml) at 60° C. for 17 hours. The reaction solution was concentrated by rotary evaporation and the residue was taken up in ethyl acetate (50 ml). Then it was washed with 0.5 N aqueous sodium hydroxide solution (50 ml) and with saturated sodium chloride solution (50 ml), and the organic phase was dried over MgSO4, filtered and concentrated under reduced pressure. This gave the product (697 mg) with a molecular weight of 274.3 g/mol (C12H19FN2O2S), MS (ESI): m/e=275 (M+H+).

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated by rotary evaporation
  2. washThen it was washed with 0.5 N aqueous sodium hydroxide solution (50 ml) and with saturated sodium chloride solution (50 ml)
  3. dry with materialthe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure