反应详情

温度

150 °C

A mixture of 0.094 g (0.18 mmol) of the product of Step B and 0.027 g (0.18 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 5 min. After the reaction vessel had cooled again to room temperature, the reaction mixture was partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was separated, washed with aq. NaHCO3, brine, dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–75% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 504.2 (M+1), 506.0 (M+3); Rt=3.39 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 vessel had cooled again to room temperature
4. customthe reaction mixture was partitioned between EtOAc and saturated aqueous NaHCO3 solution
5. customThe organic layer was separated
6. washwashed with aq. NaHCO3, brine
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified on a silica gel flash chromatography column
11. washeluted with 0–75% EtOAc-hexane
12. customEvaporation of the purified fractions
13. customdrying in vacuo