HRID1388926

反应详情

EQUATION

反应方程式

HRID 1388926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

p-Chlorobenzoyl chloride (2.75 ml, 20 mmol), dissolved 20 ml of methylene chloride and 2.6 g (20 mmol) of aluminum chloride are mixed well at room temperature. After about 5 minutes 1.87 g (10 mmole) of 2-methoxycarbonyl-4-methylthio-1-methylpyrrole is added dropwise. The reaction mixture turns immediately into a dark red colored solution. The reaction is stirred for one hour before it is diluted with 75 ml of methylene chloride and extracted with water. The methylene chloride layer is separated, washed sucessively with 25 ml sodium bicarbonate solution and 50 ml of saturated brine, dried over anhydrous sodium sulfate and concentrated to an oil. The oil is crystallized from ethanol to give 1.0 g of 5-(p-chlorobenzoyl)-2-methoxycarbonyl-4-methylthio-1-methylpyrrole.

WORKUP

后处理

  1. additionare mixed well at room temperature
  2. extractionextracted with water
  3. customThe methylene chloride layer is separated
  4. washwashed sucessively with 25 ml sodium bicarbonate solution and 50 ml of saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated to an oil
  7. customThe oil is crystallized from ethanol