HRID234828

反应详情

EQUATION

反应方程式

HRID 234828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A pyridine solution (0.4 mL) of N, N-dimethylethylenediamine (0.049 g) is added to 9-chloro-6-fluoro-4-(p-methoxybenzyloxy)benzo[g ]isoquinoline-5,10-dione of Preparative Example 29 (0.011 g) and the resultant solution is stirred under a nitrogen atmosphere for 1.75 h at room temperature. The excess amine and pyridine are removed under a slow stream of nitrogen. The residue is placed under vacuun for 3 h and purified by silica gel column chromathography commencing with 1% to 2% methanol in dichloromethane. The removal of the eluents yields 9-chloro-6-[(2-dimethylaminoethyl)amino]-4-(p-methoxybenzyloxy)benzo[g]isoquinoline-5,10-dione as a purple solid (10 mg).

WORKUP

后处理

  1. customThe excess amine and pyridine are removed under a slow stream of nitrogen
  2. custompurified by silica gel column chromathography
  3. customThe removal of the eluents