HRID1763972
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
A solution of 3-dimethylamino-1,1-diphenyl-propan-2-ol (2 55g), 4-diethylaminobutyric acid hydrochloride (1 95g) and dicyclohexylcarbodiimide (2 1g) in dichloromethane (50 ml) was stirred at room temperature for 5 days. Dicyclohexylurea was filtered off and the filtrate concentrated. The residue was dissolved in dilute hydrochloric acid and ether. The acid extract was basified; isolation through ether in the normal manner gave an oil which was chromatographed as alumina (200g.). Elution with progressively graded mixtures of light petroleum and ether gave the 4-diethylaminobutyrate of 3-dimethylamino-1,1-diphenyl-propan-2-ol isolated as the dihydrochloride (41%) as a glass.
WORKUP
后处理
- filtrationDicyclohexylurea was filtered off
- concentrationthe filtrate concentrated
- dissolutionThe residue was dissolved in dilute hydrochloric acid
- extractionThe acid extract
- customisolation through ether in the normal manner gave an oil which
- customwas chromatographed as alumina (200g.)
- washElution with progressively graded mixtures of light petroleum and ether