HRID653833

反应详情

EQUATION

反应方程式

HRID 653833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6 g (15 mmol) of 1-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)-2-(4-ethoxycarbonylphenoxy)ethanone (from Example 5) were stirred with 5 g of potassium hydroxide in 90 ml of ethanol/water/dimethyl sulfoxide (5:3:1) at 80° C. for 5 min and poured into ice-water, the alkaline solution was extracted with ether and the extract was discarded, and then the pH was adjusted to 3 with concentrated hydrochloric acid, and the acid solution was extracted with ethyl acetate. The latter extract was washed with water, dried over magnesium sulfate and evaporated. Recrystallization of the residue from ethanol provided 2.8 g of the title compound of melting point 168°-170° C.

WORKUP

后处理

  1. extractionthe alkaline solution was extracted with ether
  2. extractionthe acid solution was extracted with ethyl acetate
  3. extractionThe latter extract
  4. washwas washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customRecrystallization of the residue from ethanol