反应详情

温度

100 °C

To a stirred solution of (4,6-dichloro-pyrimidin-5-yl)acetaldehyde (Preparation 208, 2 g, 10.5 mmol) and 1-Amino-cyclopropane-carboxylicacidmethylester hydrochloride (1.33 g, 11.6 mmol) in ethanol (30 mL) was added triethylamine (4.4 mL, 31.6 mmol) and the mixture heated in a sealed tube at 100° C. for 10 hours. Acetic acid (1.21 mL, 21.1 mmol) was then added and the mixture heated at 100° C. for additional 16 hours. The reaction mixture was cooled to room temperature and diluted with DCM (200 mL). The organic layer was washed with water (2×50 mL), brine (50 mL), dried (Na2SO4) and evaporated in vacuo. The crude material was purified by column chromatography on silica gel (gradient of hexane:EtOAc 100:0 to 90:10) to afford the title compound as a solid in 35% yield, 900 mg.

1. temperaturethe mixture heated at 100° C. for additional 16 hours
2. temperatureThe reaction mixture was cooled to room temperature
3. washThe organic layer was washed with water (2×50 mL), brine (50 mL)
4. dry with materialdried (Na2SO4)
5. customevaporated in vacuo
6. customThe crude material was purified by column chromatography on silica gel (gradient of hexane:EtOAc 100:0 to 90:10)