HRID27781

反应详情

EQUATION

反应方程式

HRID 27781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe resulting mixture was concentrated to dryness
  2. dissolutionthe residue was dissolved in dimethylformamide
  3. addition1.6 g of cyclohexanecarboxylic acid chloride was added to the solution
  4. additionThe reaction mixture was poured into ice-water
  5. extractionthe mixture was extracted with chloroform
  6. additionA mixture of diethyl ether and petroleum benzene
  7. additionwas added to the
  8. extractionextract