反应详情

温度

80 °C

6-Methyl-pyrimidin-4-yl amine (545 mg) was suspended in DCE (5 mL) and chloroacetylchloride (0.4 mL) was added dropwise. The reaction was heated in a microwave at 80° C. for 5 mins. The reaction mixture was cooled, filtered and a solid obtained. The reaction was repeated a second time and both batches of solid were combined, washed with dichloromethane then suspended in dichloromethane and sat. NaHCO3 (aq.) was added. The organic phase was collected and the aqueous layer extracted with dichloromethane (×2). The combined organic layer was dried over sodium sulphate and concentrated. The crude product was purified by silica gel chromatography eluting with 0-10% MeOH/dichloromethane to give the sub-titled compound as a yellow solid (120 mg).

1. temperatureThe reaction mixture was cooled
2. filtrationfiltered
3. customa solid obtained
4. washwashed with dichloromethane
5. additionsat. NaHCO3 (aq.) was added
6. customThe organic phase was collected
7. extractionthe aqueous layer extracted with dichloromethane (×2)
8. dry with materialThe combined organic layer was dried over sodium sulphate
9. concentrationconcentrated
10. customThe crude product was purified by silica gel chromatography
11. washeluting with 0-10% MeOH/dichloromethane