HRID2300972

反应详情

EQUATION

反应方程式

HRID 2300972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

115 g of N-tert.-butyl-2-methoxycarbonyl-5-nitrobenzenesulfonamide (Example c) in 1500 ml of methanol are gassed with about 200 g of dimethylamine. The mixture is stirred at about 35° C. for one week. The solution is concentrated under reduced pressure, the residue is taken up in ethyl acetate and the mixture is washed successively with dilute hydrochloric acid, saturated NaHCO3 solution and saturated NaCl solution. After drying over MgSO4, the organic phase is concentrated. 92 g of N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzensulfonamide are obtained: m.p.: 138-141° C.

WORKUP

后处理

  1. concentrationThe solution is concentrated under reduced pressure
  2. washthe mixture is washed successively with dilute hydrochloric acid, saturated NaHCO3 solution and saturated NaCl solution
  3. dry with materialAfter drying over MgSO4
  4. concentrationthe organic phase is concentrated