反应详情

A solution of 10-(p-methoxybenzyloxy)-5-chloro-2-methylisoquino[5,6,7-cd]indazole-6(2H)-one of Example 11 (0.053 g) and N,N-dimethylethylenediamine (0,115 g) in pyridine (0.5 mL) is heated at 120° C. for 3.5 h under a nitrogen atmosphere. The excess diamine and pyridine are removed by a slow stream of nitrogen gas and the resultant dark orange residue is placed under vacuo for 3 h. The crude material is purified by radial chromathography (silica gel, 2 mm thickness) using gradient elution commencing with 2% methanol/98% chloroform (100 mL) to mixtures containing 4% methanol (75 mL) to 6% methanol (60 mL). Upon removal of the 4% methanol (96% chloroform eluent, starting material is recovered (10 mg). Removal of the 6% methanol/94% chloroform eluent led to 10-p-methoxybenzyloxy-5-[[2-(dimethylamino)ethyl]amino]-2-methylisoquino[5,6,7-cd]indazole-6(2H)-one as a pure product (22 mg).

1. customThe excess diamine and pyridine are removed by a slow stream of nitrogen gas
2. customThe crude material is purified by radial chromathography (silica gel, 2 mm thickness)
3. washgradient elution
4. additioncontaining 4% methanol (75 mL) to 6% methanol (60 mL)
5. customUpon removal of the 4% methanol (96% chloroform eluent
6. customis recovered (10 mg)
7. customRemoval of the 6% methanol/94% chloroform eluent