反应详情

温度

80 °C

(3R,5S)-3,5-bis-(tert-Butoxycarbonylamino)-piperidine (4) (1.68 g, 5.33 mmol) was suspended in DMF (20 mL), sonicated for 2 minutes and added to the crude reaction mixture containing N-[2-benzyloxy-4-(4,6-dichloro-[1,3,5]triazin-2-ylamino)-phenyl]-acetamide (400). The mixture was heated to 80° C. for 8 h. LC-MS indicated complete reaction at this point. The mixture was concentrated to a volume of 50 mL and poured into ice-water. A white solid precipitated immediately and was collected by filtration under reduced pressure followed by drying under high vacuum for 16 h to give the desired product (401) as a white powder (2.32 g, 2.4 mmol, 95% total yield for two steps). LC-MS (ESI): (exact mass: 961.54) m/e=962.7 [M+1]+ (100%).

1. customsonicated for 2 minutes
2. additionadded to the crude
3. customreaction mixture
4. customreaction at this point
5. concentrationThe mixture was concentrated to a volume of 50 mL
6. additionpoured into ice-water
7. customA white solid precipitated immediately
8. filtrationwas collected by filtration under reduced pressure
9. customby drying under high vacuum for 16 h