HRID653833
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionthe alkaline solution was extracted with ether
- extractionthe acid solution was extracted with ethyl acetate
- extractionThe latter extract
- washwas washed with water
- dry with materialdried over magnesium sulfate
- customevaporated
- customRecrystallization of the residue from ethanol