反应详情

温度

80 °C

A mixture of 1-ethyl-3-methyl-4-chloro-1H-pyrazolo[3,4-b]quinoline (1.0 g, 4.3 mmol), DMSO (3 ml) and benzylamine (0.98 ml, 9 mmol) is heated at 80° C. overnight. The reaction mixture is poured into water (100 ml), then NH4OH (0.5 ml) is added. The mixture is extracted with CH2Cl2 (200 ml) and the CH2Cl2 is concentrated to about 20 ml, and then this solution is purified by column chromatography on silica gel, followed by high pressure liquid chromatography eluting with 20% ethyl acetate/hexane to afford the product as the free base. The free base is dissolved in CH2Cl2 (20 ml) and treated with ethereal HCl. The mixture is evaporated and the residue is crystallized from ether to afford 0.9 g of 1-ethyl-3-methyl-N-(phenylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine.HCl, as an off white solid, m.p. 228°-231° C.

1. extractionThe mixture is extracted with CH2Cl2 (200 ml)
2. concentrationthe CH2Cl2 is concentrated to about 20 ml
3. customthis solution is purified by column chromatography on silica gel
4. washeluting with 20% ethyl acetate/hexane
5. customto afford the product as the free base
6. customThe mixture is evaporated
7. customthe residue is crystallized from ether