反应详情

温度

95 °C

A stirred mixture of 2-(2-chloro-5-methylpyrimidin-4-yl)-benzo[b]thiophene-4-carboxylic acid methylamide (400 mg, 1.26 mmol) and 3-(4-methylpiperazin-1-yl)-propylamine (594 mg, 3.78 mmol) in 1,4-dioxane (6 mL) is heated at 95° C. under a nitrogen atmosphere for 60 hours. After concentration and subsequent chromatography on silica gel, eluting with 2 M NH3/MeOH in dichloromethane 0-8%, the free base of the title compound is obtained as a solid (325 mg, 59% yield). The free base (300 mg, 0.684 mmol) is dissolved in MeOH (20 mL) and dichloromethane (20 mL) and the solution is bubbled with a small stream of anhydrous HCl gas for 2 minutes. After concentration, the solid is suspended in MeOH (5 mL) and diethyl ether (20 mL), sonicated, filtered and dried at 60° C. under vacuum to give the title compound as a yellow solid (311 mg, 83% yield). ES+(m/z) 439 [M(free base)+H].

1. concentrationAfter concentration and subsequent chromatography on silica gel
2. washeluting with 2 M NH3/MeOH in dichloromethane 0-8%