反応 #56059

反応方程式

5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxy-3,4-dihydrocarbostyril hydrochloride

sodium methylate

carbostyril

→

8-cyclohexylcarbonyloxy-5-(1-hydroxy-2-isopropylaminobutyl)-3,4-dihydrocarbostyril

溶媒

methanol

反応条件

後処理

1. 1
   濃縮The resulting mixture was concentrated to dryness
2. 2
   workup.DISSOLUTIONthe residue was dissolved in dimethylformamide
3. 3
   workup.ADDITION1.6 g of cyclohexanecarboxylic acid chloride was added to the solution
4. 4
   workup.ADDITIONThe reaction mixture was poured into ice-water
5. 5
   抽出the mixture was extracted with chloroform
6. 6
   workup.ADDITIONA mixture of diethyl ether and petroleum benzene
7. 7
   workup.ADDITIONwas added to the
8. 8
   抽出extract

実験手順

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).

出典