HRID1275209

反应详情

EQUATION

反应方程式

HRID 1275209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of ethylmagnesium bromide in ether (38.0 mL, 38.0 mmol) at 0° C., was added a solution of 3',4'-difluoroacetophenone (5.0 g, 32.0 mmol) in diethyl ether (35 mL). The reaction mixture was stirred at 0° C. for 1 h when TLC analysis indicated that the reaction was complete (Rf =0.3, 3:1 hexane/EtOAc). The reaction was quenched carefully by adding 38 mL of water. It was extracted with diethyl ether (2×30 mL), washed with Rochelle's salt followed by brine and the organic layer was dried over Na2SO4. The solvent was removed in vacuo after filtration and 2-(3,4-difluorophenyl)propan-2-ol was obtained as a colorless oil (crude wt.=5.4 g, 97%) which looked >90% pure by NMR. It was used in the next step without purification.

WORKUP

后处理

  1. customThe reaction was quenched carefully
  2. additionby adding 38 mL of water
  3. extractionIt was extracted with diethyl ether (2×30 mL)
  4. washwashed with Rochelle's salt
  5. dry with materialthe organic layer was dried over Na2SO4
  6. customThe solvent was removed in vacuo
  7. filtrationafter filtration