HRID2261436

反应详情

EQUATION

反应方程式

HRID 2261436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a suspension of LiAlH4 (155 mg, 4.0 mmol) in THF (25 mL) a solution of 3-(4-hydroxymethyl-phenyl)-propionic acid (720 mg, 4.0 mmol) in THF (20 mL) is added within 2 min. The resulting mixture is stirred at 70° C. for 80 min before it is treated with sat. aq. NH4Cl solution (10 mL). The suspension is filtered over celite, the filtrate is diluted with water (200 mL) and extracted with diethyl ether (2×75 mL) followed by EA (2×75 mL). The organic extracts are combined, dried over Na2SO4 and evaporated to leave 3-(4-hydroxymethyl-phenyl)-propan-1-ol (0.51 g) as a colourless oil; tR=0.61 min.

WORKUP

后处理

  1. additionis added within 2 min
  2. filtrationThe suspension is filtered over celite
  3. additionthe filtrate is diluted with water (200 mL)
  4. extractionextracted with diethyl ether (2×75 mL)
  5. dry with materialdried over Na2SO4
  6. customevaporated