反应 #674288

反应方程式

NH4Cl

NaBH4

2′,6′-dichloro-5′-fluoroacetophenone

NaBH4

→

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

收率 105.2%

溶剂

MeOH

反应条件

后处理

1. 1
   温度to warm to room temperature
2. 2
   workup.STIRRINGstirred at room temperature for 30 min
3. 3
   浓缩The reaction solution was concentrated
4. 4
   其他to remove the solvent
5. 5
   其他to give the residue
6. 6
   萃取The aqueous phase was then extracted with EtOAc (3×65 mL)
7. 7
   洗涤The combined organic phase was washed with H2O (50 mL) and brine (50 mL)
8. 8
   干燥dried over anhydrous Na2SO4
9. 9
   浓缩concentrated by evaporation in vacuo

实验过程

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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