反应详情

温度

85 °C

3.36 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxycarbostyril hydrochloride was dissolved in 20 ml of trifluoroacetic acid, and 8.8 g of cyclohexanecarboxylic acid chloride was added to the solution. The mixture was then heated at a temperature of 85° C. while refluxing. The reaction mixture was concentrated and diethyl ether was added to the residue to crystallize the product. The crystals thus obtained were separated by filtration and washed with diethyl ether. The resulting crystals were extracted successively with a saturated aqueous solution of sodium bicarbonate and chloroform, and the organic layer was washed with water, dried and concentrated to dryness. The resulting residue was crystallized from a mixture of diethyl ether and petroleum benzene to obtain 3.59 g of 5-(1-cyclohexylcarbonyloxy-2-isopropylaminobutyl)-8-cyclohexylcarbonyloxycarbostyril having a melting point of 162° to 163° C. (after recrystallization from chloroform-n-hexane).

1. temperaturewhile refluxing
2. concentrationThe reaction mixture was concentrated
3. additiondiethyl ether was added to the residue
4. customto crystallize the product
5. customThe crystals thus obtained
6. customwere separated by filtration
7. washwashed with diethyl ether
8. extractionThe resulting crystals were extracted successively with a saturated aqueous solution of sodium bicarbonate and chloroform
9. washthe organic layer was washed with water
10. customdried
11. concentrationconcentrated to dryness
12. customThe resulting residue was crystallized from a mixture of diethyl ether and petroleum benzene