HRID1194784

反应详情

EQUATION

反应方程式

HRID 1194784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21.7 g of 2-acetyl-4,5,6,7-tetrahydro-4,4,7,7-tetramethylbenzo[b]thiophene are dissolved in 250 ml of ethanol and the solution is treated gradually with 5.5 g of sodium borohydride. The mixture is left to come to room temperature and is stirred for a further 2 hours. The mixture is poured on to ice, extracted with ether, the organic phase is washed once with saturated sodium chloride solution, dried and evaporated. The crude product is filtered over silica gel (eluting agent hexane/ether 3:1) and recrystallized from hexane. There are obtained 20.2 g of 4,5,6,7-tetrahydro-α,4,4,7,7-pentamethylbenzo[b]thiophene-methanol in the form of colorless crystals, m.p. 53°-55° C.

WORKUP

后处理

  1. waitThe mixture is left
  2. customto come to room temperature
  3. additionThe mixture is poured on to ice
  4. extractionextracted with ether
  5. washthe organic phase is washed once with saturated sodium chloride solution
  6. customdried
  7. customevaporated
  8. filtrationThe crude product is filtered over silica gel (eluting agent hexane/ether 3:1)
  9. customrecrystallized from hexane