HRID67177

反应详情

EQUATION

反应方程式

HRID 67177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 10.9 g of ethyl 4-formyl-1,2,5-trimethylpyrrole-3-carboxylate in 40 ml of methanol is added dropwise under nitrogen 5.6 g of sodium borohydride in methanol while maintaining the reaction temperature below 50° C. after total addition the reaction mixture is stirred at ambient temperature for 4 hours, then 90 ml of water introduced and the reaction mixture saturated with potassium carbonate and extracted with ether. The combined ether extracts are dried and concentrated in vacuo leaving a yellow solid which is recrystallized from cyclohexane to give ethyl 4-(hydroxymethyl)-1,2,5-trimethylpyrrole-3-carboxylate, mp 184°-186° C.

WORKUP

后处理

  1. temperaturewhile maintaining the reaction temperature below 50° C.
  2. additionafter total addition the reaction mixture
  3. extractionthe reaction mixture saturated with potassium carbonate and extracted with ether
  4. dry with materialThe combined ether extracts are dried
  5. concentrationconcentrated in vacuo
  6. customleaving a yellow solid which
  7. customis recrystallized from cyclohexane