HRID69086

反应详情

EQUATION

反应方程式

HRID 69086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of methyl 4-methylthiophene-2-carboxylate (2.7 g, 6.4 mmol) in dichloromethane (20 mL) is added 48% aq. HBr (12 mL), H2SO4 (6 mL), ZnBr2 (5.4 g), and HCHO (2.2 mL, 37%) at 0-5° C. The mixture is stirred at room temperature for 16 hours. The solution is diluted with water, extracted with dichloromethane, washed with NaHCO3 solution, saturated brine solution, water, dried over sodium sulfate, and concentrated to give the title compound as an off white solid (3.5 g, 81%).

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. washwashed with NaHCO3 solution, saturated brine solution, water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated