反应详情

温度

150 °C

A mixture of 0.432 g (0.95 mmol) of the product of Step B, 250 A (1.67 mmol) of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) in 2 mL DMF was placed in a 10 mL reaction tube of a CEM Corporation Discover 300 Watt microwave reactor. The reaction vessel was sealed, placed in the microwave reactor and heated at 150° C. for 10 min. After the reaction mixture had cooled to room temperature, it was partitioned between EtOAc and 10% aq. NaHSO4 and extracted. The organic layer was washed with 10% aq. NaHSO4, water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 438.1 (M+1), 440.1 (M+3); Rt=4.72 min.

1. customwas placed in a 10 mL reaction tube of a CEM Corporation Discover 300 Watt microwave reactor
2. customThe reaction vessel was sealed
3. temperatureAfter the reaction mixture had cooled to room temperature
4. customit was partitioned between EtOAc and 10% aq. NaHSO4
5. extractionextracted
6. washThe organic layer was washed with 10% aq. NaHSO4, water, brine
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified on a silica gel flash chromatography column
11. washeluted with 0–10% EtOAc-hexane
12. customEvaporation of the purified fractions
13. customdrying in vacuo