반응 #607440

반응 방정식

3′,5′-difluoroacetophenone

sodium borohydride

→

title compound

수율 99.3%

1-(3,5-difluorophenyl)ethanol

수율 99.3%

용매

methanol

반응 조건

후처리

1. 1
   기타quenched carefully by the addition of a saturated aqueous ammonium chloride solution (150 mL)
2. 2
   추출The extraction
3. 3
   세척The combined organic layers were washed with brine (200 mL)
4. 4
   건조dried over anhydrous Na2SO4
5. 5
   여과filtered
6. 6
   기타The solvent was removed in vacuo

실험 절차

To a colorless stirred solution of 3′,5′-difluoroacetophenone (50.00 g, 320.24 mmol) in methanol (320 mL), sodium borohydride (3.41 g, 86.47 mmol, 0.27 eq) was added portion wise over 20 minutes at room temperature under inert atmosphere (Ar). Then the reaction mixture was stirred for 45 min at room temperature and then quenched carefully by the addition of a saturated aqueous ammonium chloride solution (150 mL). The extraction was carried out with ethyl acetate (2×200 mL). The combined organic layers were washed with brine (200 mL), dried over anhydrous Na2SO4 and filtered. The solvent was removed in vacuo to give the title compound (50.29 g, 99%) as a colorless oil. The alcohol was used as such in the subsequent step.

출처