反应详情

温度

60 °C

A solution of 1.43 g (10 mmol) 3-chloro-2-methyl-phenol and 0.4 g sodium hydride (60% in paraffine, 10 mmol) in 20 ml THF were stirred for 30 min at ambient temperature. After adding 1.25 g (5 mmol) 4-(2-chloro-pyrimidin-4-yloxy)-2,5-dimethyl-phenylamine the mixture was stirred for 20 hrs at 60° C. After cooling down to ambient temperature 20 ml water was added and the organic layer was separated, dried over magnesium sulfate, concentrated in vacuo, column chromatography (cycclhexane/ethyl acetate, 2:1) and a second column chromatography (dichloromethane) yielded 640 mg (30%) with a purity of 85%; log P (pH=2.3)=2.81.

1. additionwas added
2. customthe organic layer was separated
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo, column chromatography (cycclhexane/ethyl acetate, 2:1)
5. customa second column chromatography (dichloromethane) yielded 640 mg (30%) with a purity of 85%