反应详情

Dess-Martin periodinane (7 g) was added to a solution of N-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-2-(2-hydroxyethyl)-4-methoxy-benzamide (4.6 g) in methylene chloride (279 mL). The reaction mixture was stirred for 2 h at room temperature, then further Dess-Martin periodinane (1.4 g) was added, stirring for a further 4 h at room temperature. Then 5% Na2S2O3 solution was added to the reaction solution and the organic phase was then washed with water. The methylene chloride phase was dried over sodium sulfate and the solvent was removed in vacuum. The raw product was purified by preparative HPLC. In this way the product was obtained with molecular weight 396.15 (C22H21FN2O4); MS (ESI): 397 (M+H+).

1. stirringstirring for a further 4 h at room temperature
2. washthe organic phase was then washed with water
3. dry with materialThe methylene chloride phase was dried over sodium sulfate
4. customthe solvent was removed in vacuum
5. customThe raw product was purified by preparative HPLC
6. customIn this way the product was obtained with molecular weight 396.15 (C22H21FN2O4)