HRID1167710

反应详情

EQUATION

反应方程式

HRID 1167710 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 3,4-difluorobenzaldehyde (5.0 g, 35.2 mmol) in diethyl ether (35 mL)in a round bottom flask was added a solution of ethylmagnesium bromide in THF (38.0 mL, 38.0 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 1 h when TLC analysis indicated that the reaction was complete (Rf=0.5, 8:1 hexane/EtOAc). The reaction was quenched carefully by adding 38 mL of water. It was extracted with diethyl ether (2×30 mL), washed with brine and the organic layer was dried over Na2SO4. The solvent was removed in vacuo after filtration and 1-(3,4-difluorophenyl)propan-1-ol was obtained as a yellow oil (crude wt.=6.0 g) 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 brine
  5. dry with materialthe organic layer was dried over Na2SO4
  6. customThe solvent was removed in vacuo
  7. filtrationafter filtration