反应详情

温度

100 °C

Hexahydro-pyrrolo[3,4-c]pyrrole-2-carboxylic acid tert-butyl ester (1.20 g, 5.6 mmol), 2-chloro-4,6-dimethyl-pyrimidine (1.03 g, 7.2 mmol), Cs2CO3 (2.12 g, 6.5 mmol) and DMF (15 mL) were combined and heated to 100° C. for 24 hours. The reaction was then allowed to cool and water and EtOAc were added. The products were extracted into EtOAc, dried over Na2SO4, and concentrated. The resulting crude mixture was purified by flash column chromatography (EA/hex) to give the title compound (1.27 g, 71%). MS (ESI) mass calcd. for C17H26N4O2, 318.42; m/z found, 319.2 [M+H]+. 1H NMR (400 MHz, CDCl3): 6.25 (s, 1H), 3.85-3.75 (m, 2H), 3.69-3.46 (m, 4H), 3.38-3.20 (m, 2H), 2.94 (br s, 2H), 2.29 (s, 6H), 1.44 (s, 9H).

1. temperatureto cool
2. extractionThe products were extracted into EtOAc
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customThe resulting crude mixture was purified by flash column chromatography (EA/hex)