반응 #83239

반응 방정식

4,7-dihydro-6-ethoxycarbonyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-7-oxopyrazolo[1,5-a]pyrimidine

lithium borohydride

→

6-ethoxycarbonyl-2-(4-fluorophenyl)-7-oxo-3-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine

수율 39.8%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도the mixture was refluxed for 1 hour
2. 2
   온도After cooling
3. 3
   기타the reaction mixture was quenched with an aqueous saturated ammonium chloride solution
4. 4
   추출extracted with ethyl acetate
5. 5
   세척The extracts were washed with brine
6. 6
   기타dried
7. 7
   농축concentrated in vacuo
8. 8
   기타The residue was crystallized from ethanol

실험 절차

To a mixture of 4,7-dihydro-6-ethoxycarbonyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-7-oxopyrazolo[1,5-a]pyrimidine (100 mg) in tetrahydrofuran (4 ml) was added lithium borohydride (2 mole in tetrahydrofuran, 0.26 ml) at room temperature and the mixture was refluxed for 1 hour. After cooling, the reaction mixture was quenched with an aqueous saturated ammonium chloride solution and extracted with ethyl acetate. The extracts were washed with brine, dried and concentrated in vacuo. The residue was crystallized from ethanol to give 6-ethoxycarbonyl-2-(4-fluorophenyl)-7-oxo-3-(pyridin-4-yl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine (40 mg).

출처