HRID2294714

反应详情

EQUATION

反应方程式

HRID 2294714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.11 g (9.4 mmol) of ethyl (RS)-α-(sulphonylmethyl)hydrocinnamate guanidine salt in 400 ml of semi-concentrated hydrochloric acid is heated to reflux for 20 hours. Subsequently, the reaction solution is evaporated under reduced pressure and, for purification, the residue obtained is chromatographed on 50 g of silica gel using a 9:1 to 1:1 mixture of water and methanol as the eluent. After lyophilization from water there is obtained 0.6 g of (RS)-α-(sulphonylmethyl)hydrocinnamic acid guanidine salt as a colourless powder, MS: 243 (M-H)-.

WORKUP

后处理

  1. temperatureto reflux for 20 hours
  2. customSubsequently, the reaction solution is evaporated under reduced pressure and, for purification
  3. customthe residue obtained
  4. customis chromatographed on 50 g of silica gel using a 9:1
  5. additionto 1:1 mixture of water and methanol as the eluent