反应详情

温度

90 °C

(3-Chloro-benzyl)-[6-(4-chloromethyl-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-amine (150 mg, 0.35 mmol) is suspended in 5 ml dioxane and treated with N-ethyl-piperazine. The mixture is heated to 90° C. for 7 h. The solvent is evaporated and the residue is purified by flash chromatography on 34 g of silica gel. The column is eluted using a mixture of dichloromethane/methanol with gradually increasing concentrations of methanol starting with 100:1.25 and ending with 100:5 and then switching to dichloromethane/methanol/conc. ammonia starting with 100:5:0.25 and ending with 100:10:0.5. Fractions containing the title compound were pooled and concentrated on a rotary evaporator to give the title compound; m.p. 241-243° C.; MS-ES+: (M+H)+=461.

1. customThe solvent is evaporated
2. customthe residue is purified by flash chromatography on 34 g of silica gel
3. washThe column is eluted
4. additiona mixture of dichloromethane/methanol
5. temperaturewith gradually increasing concentrations of methanol starting with 100:1.25
6. additionFractions containing the title compound
7. concentrationconcentrated on a rotary evaporator