HRID1351611

反应详情

EQUATION

反应方程式

HRID 1351611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred mixture of 4-chloro-2-(methylthio)pyrimidine-5-carbonitrile (0.843 g, 4.54 mmol) and zinc dust (1.48 g, 22.71 mmol) in ethanol (7.5 mL) and water (1.4 mL) was slowly added acetic acid (0.29 mL, 5.13 mmol). The resulting reaction mixture was vigorously stirred for 3 h. The solids were removed by filtration and the filtrate concentrated in vacuo. The residue was chromatographed on silica gel 60 (35 g), eluting with 10:1-20:89-70 CH2Cl2:2-propanol:hexane to give the title compound. M.S. (M+1): 152.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. customThe solids were removed by filtration
  3. concentrationthe filtrate concentrated in vacuo
  4. customThe residue was chromatographed on silica gel 60 (35 g)
  5. washeluting with 10:1-20:89-70 CH2Cl2