HRID972940

反应详情

EQUATION

反应方程式

HRID 972940 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
24 °C

PROCEDURE

实验过程

A solution of 504 mg. of 1-methoxy-4-(1-hydroxy-1-methylethyl)-1,4-cyclohexadiene and 708 mg. of 5-(1,1-dimethylheptyl)resorcinol in 25 ml. of benzene was stirred at 24° C. while 5 ml. of boron trifluoride diethyl etherate was added in one portion. The reaction mixture was stirred at 24° C. for five hours. The reaction mixture then was added to 20 ml. of 6N hydrochloric acid solution. After allowing the benzene solvent to evaporated from the aqueous acid solution, the solution was extracted several times with diethyl ether. The ethereal extracts were combined, washed with water and with aqueous sodium bicarbonate solution, and dried. Evaporation of the solvent under reduced pressure provided an oil, which was crystallized from hexane to afford dl-cis-1-hydroxy-3-(1,1-dimethylheptyl)-6,6-dimethyl-6,6a,7,8,10,10a-hexahydro-9H-dibenzo[b,d]pyran-9-one.

WORKUP

后处理

  1. additionThe reaction mixture then was added to 20 ml
  2. customto evaporated from the aqueous acid solution
  3. extractionthe solution was extracted several times with diethyl ether
  4. washwashed with water and with aqueous sodium bicarbonate solution
  5. customdried
  6. customEvaporation of the solvent under reduced pressure
  7. customprovided an oil, which
  8. customwas crystallized from hexane