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
CONDITIONS
反应条件
- 温度
- 10 °C
PROCEDURE
实验过程
3.28 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxy-3,4-dihydrocarbostyril hydrochloride was dissolved in 50 ml of methanol, and a 10% methanolic solution of sodium methylate was added to the solution in an amount of 2 moles per mole of the starting carbostyril compound. The resulting mixture was concentrated to dryness, and the residue was dissolved in dimethylformamide. 1.6 g of cyclohexanecarboxylic acid chloride was added to the solution and the mixture was stirred for 2 hours at a temperature of 10° C. The reaction mixture was poured into ice-water and the mixture was extracted with chloroform. A mixture of diethyl ether and petroleum benzene was added to the extract to obtain 1.2 g of crystalline 8-cyclohexylcarbonyloxy-5-(1-hydroxy-2-isopropylaminobutyl)-3,4-dihydrocarbostyril having a melting point of 148°-149° C. (after recrystallization from chloroform-n-hexane).
WORKUP
后处理
- concentrationThe resulting mixture was concentrated to dryness
- dissolutionthe residue was dissolved in dimethylformamide
- addition1.6 g of cyclohexanecarboxylic acid chloride was added to the solution
- additionThe reaction mixture was poured into ice-water
- extractionthe mixture was extracted with chloroform
- additionA mixture of diethyl ether and petroleum benzene
- additionwas added to the
- extractionextract