HRID1010629

反应详情

EQUATION

反应方程式

HRID 1010629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred suspension of 1-Benzoyl-3-(3-bromo-5-iodophenyl)-thiourea (20.70 g, 0.0449 mol) in methanol (303 ml) was treated with sodium methoxide (2.42 g, 0.0449 mol) and stirred at ambient temperature for 4 h. The resultant suspension was evaporated to dryness at reduced pressure. The residue was mixed with water (500 ml) and extracted with ethyl acetate (3×200 ml) which was dried (MgSO4) and the solvent removed in vacuo to give a residue which was triturated with 40-60° petroleum ether/diethyl ether (1:1) to afford (3-Bromo-5-iodophenyl)-thiourea as an off-white solid (14.35 g, 89%).

WORKUP

后处理

  1. customThe resultant suspension was evaporated to dryness at reduced pressure
  2. additionThe residue was mixed with water (500 ml)
  3. extractionextracted with ethyl acetate (3×200 ml) which
  4. dry with materialwas dried (MgSO4)
  5. customthe solvent removed in vacuo
  6. customto give a residue which
  7. customwas triturated with 40-60° petroleum ether/diethyl ether (1:1)