反应详情

A solution of intermediate D40 (27 g, 5.636 mmol) and KOH (2.433 g, 43.357 mmol) in isopropyl alcohol (13.5 ml) and water (27 ml) was heated at 180° C. under microwave irradiation for 60 min. After cooling to r.t., the mixture was washed with water and NaCl (aqueous saturated solution). The organic phase was dried (Na2SO4) and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 10% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D41 as a yellow solid (1.041. g, 84%). M.P. 219.5° C.

1. washthe mixture was washed with water and NaCl (aqueous saturated solution)
2. dry with materialThe organic phase was dried (Na2SO4)
3. customthe solvent evaporated in vacuo
4. customThe crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 10% as eluent)
5. customThe desired fractions were collected
6. concentrationconcentrated in vacuo
7. customto yield intermediate compound D41 as a yellow solid (1.041. g, 84%)