反应详情

Ethyl 1-[5-[7-bromo-2-(ethylcarbamoylamino)-1,3-benzothiazol-5-yl]pyrimidin-2-yl]-4-methyl-piperidine-4-carboxylate (Jubilant) (3.0 g, 5.48 mmol) was suspended in EtOH (120 mL). N-methylmorpholine (3.0 mL, 27.4 mmol), aqueous formaldehyde (4.45 mL, 54.8 mmol) and methylamine solution (2 M) (13.7 mL, 27.4 mmol) were added and the reaction mixture stirred at rt for 16 h, followed by a further 4 hrs at 80° C. The reaction mixture was cooled to rt and the resulting precipitate filtered. The precipitate was washed with EtOH, Et2O and dried using a vacuum oven to afford the desired product (2.5 g, off white solid).

1. waitfollowed by a further 4 hrs at 80° C
2. temperatureThe reaction mixture was cooled to rt
3. filtrationthe resulting precipitate filtered
4. washThe precipitate was washed with EtOH, Et2O
5. customdried