HRID1887166

反应详情

EQUATION

反应方程式

HRID 1887166 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

To a solution of 4-[6-(4-cyclopropylmethyl-piperazin-1-yl)-pyridin-3-yl]-benzonitrile (2.0 g 6.3 mmol) dissolved in THF (40 mL) was added DIBAL-H (25 mL, 1 N) at −40° C. The mixture was stirred 2 h at −40° C. and then CH3OH (15 mL), water (100 mL) and 1 N NaOH (15 mL) was added at −40° C. The mixture was extracted with EtOAc (3×300 mL). The combined organic extracts were washed with water (3×50 mL), dried (Na2SO4) and concentrated under reduced pressure to give 1.7 g (51%) of 4-[6-(4-cyclopropylmethyl-piperazin-1-yl)-pyridin-3-yl]-benzaldehyde.

WORKUP

后处理

  1. extractionThe mixture was extracted with EtOAc (3×300 mL)
  2. washThe combined organic extracts were washed with water (3×50 mL)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated under reduced pressure