反应详情

p-Nitrophenyl chloroformate [7693-46-1] (0.339 mmol) was added to a solution of 6-(4-chloro-phenyl)-2-(2,4-dimethoxy-pyrimidin-5-yl)-1-isopropyl-5-piperidin-4-yl-5,6-dihydro-1H-pyrrolo[3,4-b]pyrrol-4-one (Example 106) (0.242 mmol) and Et3N (0.726 mmol) in CH2Cl2 (2 mL). After stirring at rt for 30 min, the reaction mixture was treated with methylamine (2M/THF) (3.63 mmol) and warmed to 35° C. After 20 h, the reaction mixture was diluted with EtOAc and washed with a saturated aqueous solution of NaHCO3 (3×). The organic phase was dried (MgSO4), filtered and concentrated. The residue was purified using a RediSep® silica gel column to afford the title compound as a white solid. tR: 4.93 min (HPLC 4); ESI-MS: tR=0.98 min, [M+H]+ 553/555 (LC-MS 1).

1. temperaturewarmed to 35° C
2. waitAfter 20 h
3. washwashed with a saturated aqueous solution of NaHCO3 (3×)
4. dry with materialThe organic phase was dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified