HRID131418

反应详情

EQUATION

反应方程式

HRID 131418 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine 2-Isopropyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine (0.969 g, 3.85 mmol) and (S)-2-(2-methoxy-ethyl)-piperazine (0.556 g, 3.85 mmol) in NMP (7.0 mL) and heat at 200° C. for 4 hours. Cool to ambient temperature and dilute with water. Extract with ethyl acetate to give 1.51 g of the crude product. Silica gel chromatography, eluting with methylene chloride: 2N NH3/methanol (100:4), gives 0.560 g of the title compound as a tan solid: mp=158-160° C.; mass spectrum (ion spray): m/z=379 (M+1); Analysis for C23H30N4O(0.2H2O): calcd: C, 72.29; H, 8.02; N, 14.66; found: C, 72.20; H, 7.70; N, 14.60.

WORKUP

后处理

  1. extractionExtract with ethyl acetate
  2. customto give 1.51 g of the crude product
  3. washSilica gel chromatography, eluting with methylene chloride