تفاعل #54310

معادلة التفاعل

8-amino-5-hydroxy-3,4-dihydrocarbostyril

cyclohexylcarbonyl chloride

→

8-cyclohexylcarbonylamino-5-hydroxy-3,4-dihydrocarbostyril

المردود 38.1%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGby stirring at 50° C. for 30 minutes
2. 2
   ترشيحThe precipitated crystals were recovered by filtration
3. 3
   غسيلwashed with ethanol
4. 4
   أخرىdried
5. 5
   workup.DISSOLUTIONdissolved in 200 ml of a 10% aqueous sodium hydroxide solution
6. 6
   workup.ADDITIONActivated carbon was added to the solution
7. 7
   workup.STIRRINGthe mixture was stirred
8. 8
   ترشيحfiltered
9. 9
   ترشيحthe precipitated crystals were recovered by filtration
10. 10
    غسيلwashed with water
11. 11
    أخرىdried
12. 12
    أخرىRecrystallization from methanol

الإجراء التجريبي

10.7 g of 8-amino-5-hydroxy-3,4-dihydrocarbostyril was dissolved in 100 ml of pyridine, and 10.0 g of cyclohexylcarbonyl chloride was added to the solution while vigorously stirring at room temperature followed by stirring at 50° C. for 30 minutes. The precipitated crystals were recovered by filtration, washed with ethanol, dried and dissolved in 200 ml of a 10% aqueous sodium hydroxide solution. Activated carbon was added to the solution, and the mixture was stirred and filtered. The filtrate was rendered acidic with hydrochloric acid under ice cooling, and the precipitated crystals were recovered by filtration, washed with water and dried. Recrystallization from methanol yielded 6.6 g of 8-cyclohexylcarbonylamino-5-hydroxy-3,4-dihydrocarbostyril as colorless amorphous crystals having a melting point of 304.2°-304.8° C.

المصدر