反应详情

To a solution of 8.86 g (20 mmol) 5-chloro-2-(2,5-dimethyl-4-nitrophenoxy)-N-ethyl-N-methylpyrimidin-4-amine in 50 ml hydrochloric acid and 50 ml methanol 13.5 g (60 mmol) tin-(II)-dichloro dihydrate was added and the mixture was refluxed for 4 h. After cooling down to ambient temperature the formed precipitate was filtered by suction, solved in water and brought to pH 8 with aqueous solution of sodium hydroxide. Ethyl acetate was added and the organic layer was separated, dried over magnesium sulfate, concentrated in vacuo and column chromatography (cyclohexane/ethyl acetate, 1:1) yielded 4.6 g (72%) with a purity of 96% log P (pH=2.3)=1.88.

1. temperaturethe mixture was refluxed for 4 h
2. filtrationwas filtered by suction
3. additionEthyl acetate was added
4. customthe organic layer was separated
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo and column chromatography (cyclohexane/ethyl acetate, 1:1)
7. customyielded 4.6 g (72%) with a purity of 96% log P (pH=2.3)=1.88