Реакция #674288

Уравнение реакции

NH4Cl

NaBH4

2′,6′-dichloro-5′-fluoroacetophenone

NaBH4

→

(±)1-(2,6-dichloro-3-fluorophenyl)ethanol

Выход 105.2%

Растворители

MeOH

Условия реакции

Обработка

1. 1
   Температураto warm to room temperature
2. 2
   workup.STIRRINGstirred at room temperature for 30 min
3. 3
   КонцентрированиеThe reaction solution was concentrated
4. 4
   Другоеto remove the solvent
5. 5
   Другоеto give the residue
6. 6
   ЭкстракцияThe aqueous phase was then extracted with EtOAc (3×65 mL)
7. 7
   ПромывкаThe combined organic phase was washed with H2O (50 mL) and brine (50 mL)
8. 8
   Сушкаdried over anhydrous Na2SO4
9. 9
   Концентрированиеconcentrated by evaporation in vacuo

Методика

To a solution of 2′,6′-dichloro-5′-fluoroacetophenone (10.4 g, 50 mmol) in MeOH (anhydrous, 80 mL) was added NaBH4 (3.78 g, 100 mmol) in portions at 0° C. After the addition of NaBH4, the solution was stirred at 0° C. for 10 min, then allowed to warm to room temperature and stirred at room temperature for 30 min. The reaction solution was concentrated to remove the solvent to give the residue. A saturated solution of NH4Cl (60 mL) was added slowly. The aqueous phase was then extracted with EtOAc (3×65 mL). The combined organic phase was washed with H2O (50 mL) and brine (50 mL), dried over anhydrous Na2SO4, concentrated by evaporation in vacuo to afford (±)1-(2,6-dichloro-3-fluorophenyl)ethanol (11 g, 100%) as a colorless oil.

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