反应详情

温度

90 °C

[2-Chloro-6-[(3S)-3-methylmorpholin-4-yl]pyrimidin-4-yl]methanol (500 mg) was dissolved in an 18% DMF in a mixture of 7:3:2 DME:water:ethanol (10 mL). 3-(1,2-Oxazol-3-yl)-1-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]urea (811 mg) and 2M aqueous sodium carbonate solution (4 mL) were then added to the solution and the resultant mixture degassed for 5 min. Dichlorobis(triphenylphosphine) palladium catalyst (73 mg) was added and the solution refluxed at 90° C. for 7 h under nitrogen atmosphere. The reaction was allowed to cool then neutralised with concentrated hydrochloric acid and loaded directly onto a SCX-2 column (50 g), the column was washed with methanol and the product eluted with 7N ammonia in methanol. The material was further purified by chromatography on silica, eluting with 5% methanol in DCM, to give the desired material (318 mg) as a white solid.

1. customthe resultant mixture degassed for 5 min
2. additionDichlorobis(triphenylphosphine) palladium catalyst (73 mg) was added
3. temperatureto cool
4. washthe column was washed with methanol
5. washthe product eluted with 7N ammonia in methanol
6. customThe material was further purified by chromatography on silica
7. washeluting with 5% methanol in DCM