HRID460983

反应详情

EQUATION

反应方程式

HRID 460983 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.8 G. of 4-bromo-3,5-dimethylthiophene-2-carboxaldehyde was dissolved in 250 ml. of dry ethanol and stirred at 20° C. 0.52 G. of sodium borohydride was added and the resulting solution was stirred for 30 minutes, then poured into ice water and extracted with ethyl ether. The combined ether extracts were washed with a solution of 50% sodium carbonate and a saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. Crystallization from cold hexane yielded 4-bromo-3,5-dimethyl-2-hydroxymethylthiophene, m.p. 85°-90° C.

WORKUP

后处理

  1. extractionextracted with ethyl ether
  2. washThe combined ether extracts were washed with a solution of 50% sodium carbonate
  3. dry with materiala saturated sodium chloride solution, dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customCrystallization from cold hexane