反应详情

温度

120 °C

To a solution of tert-butyl 4-((2-(2,4-dimethoxybenzylamino)pyridin-3-yl)methylamino)piperidine-1-carboxylate (2.89 g, 6.33 mmol) in DMF (42 ml) was added CDI (1.23 g, 7.6 mmol) in portions and the reaction mixture was stirred at 120° C. for 2 hours. A further portion of CDI was added (0.82 g) was added and the reaction mixture stirred at 130° C. for 6 hours, followed by stirring at RT for 16 hours. The reaction was diluted with water and extracted with DCM. The organics were combined, dried (NaSO4) and evaporated to dryness. Purification by column chromatography (10 to 80% EtOAc in Hx) gave the desired product (1.17 g). LC/MS (10% to 99%): M/Z (M+H)+ (obs)=483; tR=3.58.

1. additionwas added
2. stirringthe reaction mixture stirred at 130° C. for 6 hours
3. stirringby stirring at RT for 16 hours
4. extractionextracted with DCM
5. dry with materialdried (NaSO4)
6. customevaporated to dryness
7. customPurification by column chromatography (10 to 80% EtOAc in Hx)