反应详情

温度

80 °C

A mixture of 5-bromo-2-(dimethylamino)pyrimidine (6.76g, 33.17mmol), 3-aminophenylboronic acid hemisultat (7.4g, 39.78mmol) potassium carbonate (13.73g, 99.49mmol), 1,3-propanediol (12ml, 166mmol) and tetrakis(triphenylphosphine)palladium(0) (0.2g) in a mixture of water (30ml) and dimethoxyethane (60ml) is heated to 80° C. under nitrogen overnight. After cooling the mixture is diluted with water and ethyl acetate and is filtered through a fluted filterpaper. The layers are separated and the aqeous phase is extracted once with ethyl acetate. The combined organic phases are dried over sodium sulfate and evaporated to dryness. The residue is triturated with a mixture of ethyl acetate and petroleum ether (1:1) to leave crystalline 2h (5.26g, 74%). Mp 115.5-117° C.

1. temperatureAfter cooling the mixture
2. filtrationis filtered through a fluted filterpaper
3. customThe layers are separated
4. extractionthe aqeous phase is extracted once with ethyl acetate
5. dry with materialThe combined organic phases are dried over sodium sulfate
6. customevaporated to dryness
7. customThe residue is triturated with a mixture of ethyl acetate and petroleum ether (1:1)