HRID1699577

反应详情

EQUATION

反应方程式

HRID 1699577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

In a mixed solvent consisting of 2 ml of dimethylformamide and 0.2 ml of water were dissolved 200 mg of 2-(3,4-diethoxyphenyl)-4-chloromethylthiazole, 73 mg of 2-acetylpyrrole, 200 mg of sodium iodide and 200 mg of sodium hydroxide. The solution was stirred at 80° C. for 4 hours. The reaction mixture was subjected to distillation to remove the solvent. To the residue were added 30 ml of dichloromethane and 20 ml of water, and phase separation was conducted. The organic layer was washed with 15 ml of a saturated aqueous sodium chloride solution, dried and subjected to distillation to remove the solvent. The residue was recrystallized from methanol to obtain 60 mg of 2-(3,4-diethoxyphenyl)-4-(2-acetyl-1-pyrrolyl)methylthiazole as white acicular crystals.

WORKUP

后处理

  1. distillationThe reaction mixture was subjected to distillation
  2. customto remove the solvent
  3. additionTo the residue were added
  4. custom30 ml of dichloromethane and 20 ml of water, and phase separation
  5. washThe organic layer was washed with 15 ml of a saturated aqueous sodium chloride solution
  6. customdried
  7. distillationsubjected to distillation
  8. customto remove the solvent
  9. customThe residue was recrystallized from methanol