HRID968286

反应详情

EQUATION

反应方程式

HRID 968286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1,1-Dimethylamino-1,3-propanediamine (0.058 ml, 0.46 mmol) was added to a suspension of 9-chloro-5-ethyl-5H-phenanthridin-6-one I-14b (100 mg, 0.39 mmol), Pd2(dba)3 (2 mg, 0.002 mmol), (3′-dicyclohexylphosphanylbiphenyl-2-yl)dimethylamine (2.5 mg, 0.005 mmol), and dibasic potassium phosphate (115 mg, 0.54 mmol) in 1,2-dimethoxyethane (5 ml). The resultant suspension was held at 23° C. for 16 hours. The reaction mixture was concentrated in vacuo and the residue was purified by flash column chromatography (10% ethyl acetate in dichloromethane) to afford 9-(3-Dimethylamino-propylamino)-5-ethyl-5H-phenanthridin-6-one 14A (19 mg, 15%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was purified by flash column chromatography (10% ethyl acetate in dichloromethane)