HRID1667477

反应详情

EQUATION

反应方程式

HRID 1667477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (150 mg, 0.578 mmol), N-[3-(aminomethyl)phenyl]-N,N-dimethylamine (102 mg, 0.679 mmol), Pd2(dba)3 (53 mg, 0.0578 mmol), rac-BINAP (112 mg, 0.180 mmol) and NaOtBu (139 mg, 1.445 mmol) in DMA (6 mL) was heated at 85° C. for 1.5 h. The mixture was allowed to cool, diluted with EtOAc and washed with water. The organic layer was washed with sat.aq. NaHCO3, brine and dried (Na2SO4). Chromatography on silica (EtOAc/hexanes) afforded 4-chloro-6-(3-dimethylamino-benzylamino)-2H-phthalazin-1-one (28 mg) as a beige solid,

WORKUP

后处理

  1. temperatureto cool
  2. washwashed with water
  3. washThe organic layer was washed with sat.aq
  4. dry with materialNaHCO3, brine and dried (Na2SO4)