HRID1792891

反应详情

EQUATION

反应方程式

HRID 1792891 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.00 g (25.3 mmol) of methyl 2-[(tert-butylamino)sulfonyl]-6-nitrobenzoate is admixed with 3.2 g of palladium on activated carbon (5%) and hydrogenated at room temperature and under atmospheric pressure for 6 h. The reaction mixture is then filtered, the filtrate is concentrated to dryness and the residue is purified by silica gel chromatography [TLC (SiO2)ethyl acetate/n-heptane 1:1; Rf=0.38] using ethyl acetate/n-heptane (1:1). Evaporation gives 6.23 g (86% of theory) of methyl 2-amino-6-[(tert-butylamino)sulfonyl]benzoate as a beige solid of melting point 132-133° C.

WORKUP

后处理

  1. filtrationThe reaction mixture is then filtered
  2. concentrationthe filtrate is concentrated to dryness
  3. customthe residue is purified by silica gel chromatography [TLC (SiO2)ethyl acetate/n-heptane 1:1; Rf=0.38]
  4. customEvaporation