HRID2373411

反应详情

EQUATION

反应方程式

HRID 2373411 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 9-chloro-2-[4-(3-pyrrolidin-1-yl-prop-1-ynyl)-phenylamino]-5H,7H benzo[b]pyrimido[4,5-d]azepin-6-one (I-47) (0.082 g, 0.19 mmol) in EtOH (5 mL) was added Pd/C (10% wt, ˜50% H2O, 0.01 g) and the mixture was placed under H2 (1 atm) and stirred for 12 h at 22° C. The reaction mixture was filtered through Celite® and the filtrate concentrated in vacuo to give crude product as a yellow oil. Purification by C-18 RP LC-MS chromatography afforded I-66 (0.046 g, 56%):

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. customPurification by C-18 RP LC-MS chromatography
  5. customafforded I-66 (0.046 g, 56%)