反应详情

温度

100 °C

To (1S,6R)-benzyl 3,8-diazabicyclo[4.2.0]octane-8-carboxylate (2.5 g, 6.9 mmol) and 2-chloro-4,6-dimethylpyrimidine (980 mg, 6.9 mmol) in DMF (35 mL) was added Cs2CO3 (9.0 g, 27.6 mmol). The reaction flask was heated to 100° C. until starting materials were consumed, cooled to rt, diluted with EtOAc and washed with H2O. The aqueous layer was back-extracted with EtOAc (1×). The combined organics were washed with brine and dried (Na2SO4) to give an oil. Purification via silica gel (15-75% EtOAc in hexanes) gave 1.6 g (63%) of the title compound as a clear oil. MS (ESI) mass calcd. C20H24N4O2, 352.44; m/z found 353.2 [M+H]+.

1. customwere consumed
2. temperaturecooled to rt
3. additiondiluted with EtOAc
4. washwashed with H2O
5. extractionThe aqueous layer was back-extracted with EtOAc (1×)
6. washThe combined organics were washed with brine
7. dry with materialdried (Na2SO4)
8. customto give an oil
9. customPurification via silica gel (15-75% EtOAc in hexanes)