تفاعل #56061

معادلة التفاعل

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

cyclohexanecarboxylic acid chloride

→

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

المردود 136.8%

المذيبات

trifluoroacetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwhile refluxing
2. 2
   تركيزThe reaction mixture was concentrated
3. 3
   workup.ADDITIONdiethyl ether was added to the residue
4. 4
   أخرىto crystallize the product
5. 5
   أخرىThe crystals thus obtained
6. 6
   أخرىwere separated by filtration
7. 7
   غسيلwashed with diethyl ether
8. 8
   استخلاصThe resulting crystals were extracted successively with a saturated aqueous solution of sodium bicarbonate and chloroform
9. 9
   غسيلthe organic layer was washed with water
10. 10
    أخرىdried
11. 11
    تركيزconcentrated to dryness
12. 12
    أخرىThe resulting residue was crystallized from a mixture of diethyl ether and petroleum benzene

الإجراء التجريبي

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).

المصدر