反应详情

To a solution of 85 (0.104 g, 0.325 mmol) and DCM (5 mL) at RT was added TEA (0.136 mL, 0.975 mmol) and CDI (0.0527 g, 0.325 mmol) and the reaction was stirred at RT for 30 min and then added to a solution of 300 (0.080 g, 0.325 mmol), TEA (0.136 ml, 0.975 mmol) and DCM (5 mL) solution and the resulting solution stirred for 4 h. The reaction mixture was poured into water and extracted with DCM. The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with DCM/MeOH (500:7) to afford 0.160 g (83.1%) of N—((S)-2-(tert-butyldimethylsilyloxy)-1-(3,4-dichlorophenyl)ethyl)-2-(1,1,1-trifluoropropan-2-ylamino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxamide (302).

1. stirringthe resulting solution stirred for 4 h
2. extractionextracted with DCM
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by SiO2 chromatography
7. washeluting with DCM/MeOH (500:7)