反应详情

温度

100 °C

To a stirred solution of 16-1 (6.8 g, 15.2 mMol) in anhydrous 1,4-dioxane (20 mL) was added hydrazine (10.8 mL, 343 mMol). The solution was heated to 100° C. in a microwave reactor for 5 minutes. The solvent was removed in vacuo and the crude residue was taken up in ethyl acetate and washed with aqueous NaHCO3 solution followed by brine. The organic layer was dried with MgSO4, filtered and concentrated in vacuo to yield 16-2 as an orange solid. LC/MS (M+1) calculated: 442.5; observed: 442.2

1. customThe solvent was removed in vacuo
2. washwashed with aqueous NaHCO3 solution
3. dry with materialThe organic layer was dried with MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo