반응 #54308

반응 방정식

hydrochloric acid

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

ethyl chlorocarbonate

→

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

수율 63.8%

용매

sodium hydroxide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added to the solution
2. 2
   workup.STIRRINGby stirring for one hour at 30° C
3. 3
   기타After completion of the reaction
4. 4
   온도cooling
5. 5
   여과the precipitated crystals were recovered by filtration
6. 6
   세척washed with water
7. 7
   기타dried
8. 8
   기타Recrystallization of the dried crystals from ethanol

실험 절차

10.7 g of 8-amino-5-hydroxy-3,4-dihydrocarbostyril hydrochloride was dissolved in 200 ml of a 10% aqueous sodium hydroxide solution, 5.4 g of ethyl chlorocarbonate was added to the solution while stirring at room temperature followed by stirring for one hour at 30° C. After completion of the reaction, the reaction mixture was rendered acidic with hydrochloric acid under ice-cooling, the precipitated crystals were recovered by filtration, washed with water and dried. Recrystallization of the dried crystals from ethanol yielded 7.95 g of 8-ethoxycarbonylamino-5-hydroxy-3,4-dihydrocarbostyril as colorless needle crystals having a melting point of 283.8°-284.6° C.

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