HRID453244

反应详情

EQUATION

反应方程式

HRID 453244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 2 L pressure jar, under inert atmosphere, 196 g (733 mmoles) of ethyl 3-(3-chlorophenyl)-4-nitrobutanoate 377 are dissolved in 200 ml of ethanol. A suspension of 200 g of predried (3×, ethanol) Raney Nickel in 700 ml of ethanol is added and the mixture hydrogenated on a Parr hydrogenator at a maximum of 20 psi H2 pressure (STRONGLY EXOTHERMIC REACTION, ice/water cooling required). The mixture is degassed, filtered on a Celite/Norite pad, and the filtrate concentrated in vacuo, to give 136.7 g of crude 378, 78% yield, used as such in the next step.

WORKUP

后处理

  1. additionis added
  2. customThe mixture is degassed
  3. filtrationfiltered on a Celite/Norite pad
  4. concentrationthe filtrate concentrated in vacuo
  5. customto give 136.7 g of crude 378, 78% yield