反应详情

温度

100 °C

2,4-Dichloropyrimidin-5-amine (25 g, 152 mmol) and morpholine-3-carboxylic acid hydrochloride (28.1 g, 168 mmol) were dissolved in DMSO (200 mL) to give a yellow suspension. To the suspension was added N,N-diisopropylethylamine (106 mL, 610 mmol) and the mixture was heated to 100° C. for 18 hours. The mixture was cooled to room temperature and poured into ice. Water was added until the total volume was 1 L. The resulting beige suspension was stirred overnight before the solid was collected on a fritted-glass funnel of medium porosity. The solid was washed with water (3×) and then dried under a stream of nitrogen overnight to afford the title compound as a light yellow solid that was used without further purification (18.6 g, 51%). ESI-MS m/z [M+H]+ calc'd for C9H9ClN4O2, 241.04. found 241.1.

1. customto give a yellow suspension
2. temperatureThe mixture was cooled to room temperature
3. additionpoured into ice
4. customwas collected on a fritted-glass funnel of medium porosity
5. washThe solid was washed with water (3×)
6. customdried under a stream of nitrogen overnight