HRID1077228

反应详情

EQUATION

反应方程式

HRID 1077228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Suspend dl-13-ethyl-3-methoxy-6-methyl-17,17-ethylenedioxygona-1,3,5(10)-triene (9.0 g) in methanol (200 ml) and concentrated hydrochloric acid (5 ml). Heat the mixture on a steam bath for 15 minutes. Remove the solvent under vacuum and partition the residue between ether and aqueous sodium bicarbonate. Remove the organic solvents and dry to obtain a gum. Recrystallize from methanol to obtain dl-13-ethyl-3-methoxy-6-methylgona-1,3,5(10)-trien-17-one (7.29 g), m.p. 115°-123°. Recrystallize from methanol to obtain an analytical sample with m.p. 123°-127°; ultraviolet absorption peak at 280 mμ (ε2,190), infrared maximum (potassium bromide) at 5.75 μ.

WORKUP

后处理

  1. temperatureHeat the mixture on a steam bath for 15 minutes
  2. customRemove the solvent under vacuum
  3. custompartition the residue between ether and aqueous sodium bicarbonate
  4. customRemove the organic solvents
  5. customdry
  6. customto obtain a gum
  7. customRecrystallize from methanol