HRID67177
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewhile maintaining the reaction temperature below 50° C.
- additionafter total addition the reaction mixture
- extractionthe reaction mixture saturated with potassium carbonate and extracted with ether
- dry with materialThe combined ether extracts are dried
- concentrationconcentrated in vacuo
- customleaving a yellow solid which
- customis recrystallized from cyclohexane