HRID545061

反应详情

EQUATION

反应方程式

HRID 545061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

To a solution of 3-nitro-phenyl-acetonitrile (3.20 g, 19.7 mmol) in MeOH (50 mL) was added Pd/C (10% wt, ˜50% H2O, 0.32 g) and the mixture was placed under H2 (80 psi) and stirred for 2 days at 22° C. The reaction mixture was filtered through Celite® and the filtrate concentrated in vacuo to give crude product as a yellow oil. The residue was purified by silica gel chromatography (ISCO, elution with 0-10% ethyl acetate in hexanes) to give xix-l-1 (1.15 g, 44%): MS m/z=133 (M−H).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Celite®
  2. concentrationthe filtrate concentrated in vacuo
  3. customto give crude product as a yellow oil
  4. customThe residue was purified by silica gel chromatography (ISCO, elution with 0-10% ethyl acetate in hexanes)
  5. customto give xix-l-1 (1.15 g, 44%)