HRID968286
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction mixture was concentrated in vacuo
- customthe residue was purified by flash column chromatography (10% ethyl acetate in dichloromethane)