反应 #56061

反应方程式

5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxycarbostyril hydrochloride

cyclohexanecarboxylic acid chloride

→

5-(1-cyclohexylcarbonyloxy-2-isopropylaminobutyl)-8-cyclohexylcarbonyloxycarbostyril

收率 136.8%

溶剂

trifluoroacetic acid

反应条件

后处理

1. 1
   温度while refluxing
2. 2
   浓缩The reaction mixture was concentrated
3. 3
   workup.ADDITIONdiethyl ether was added to the residue
4. 4
   其他to crystallize the product
5. 5
   其他The crystals thus obtained
6. 6
   其他were separated by filtration
7. 7
   洗涤washed with diethyl ether
8. 8
   萃取The resulting crystals were extracted successively with a saturated aqueous solution of sodium bicarbonate and chloroform
9. 9
   洗涤the organic layer was washed with water
10. 10
    其他dried
11. 11
    浓缩concentrated to dryness
12. 12
    其他The resulting residue was crystallized from a mixture of diethyl ether and petroleum benzene

实验过程

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).

来源