Реакция #607440

Уравнение реакции

3′,5′-difluoroacetophenone

sodium borohydride

→

title compound

Выход 99.3%

1-(3,5-difluorophenyl)ethanol

Выход 99.3%

Растворители

methanol

Условия реакции

Обработка

1. 1
   Другоеquenched carefully by the addition of a saturated aqueous ammonium chloride solution (150 mL)
2. 2
   ЭкстракцияThe extraction
3. 3
   ПромывкаThe combined organic layers were washed with brine (200 mL)
4. 4
   Сушкаdried over anhydrous Na2SO4
5. 5
   Фильтрацияfiltered
6. 6
   ДругоеThe solvent was removed in vacuo

Методика

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.

Источник