反应详情

Sodium hydride (0.40 g, 10 mmol, 60% in oil) was suspended in tetrahydrofuran (5 mL), (3-cyanobenzyl)phosphonic acid diethyl ester obtained in Preparation Example 135 (2.53 g, 10 mmol) was added dropwise under stirring at room temperature. After stirring for 1 hour at 60° C., the solution was allowed to room temperature, acetone (0.92 g, 20 mmol) was added dropwise, and the solution was further stirred for 30 minutes at room temperature. Water (100 mL) was added to the reaction solution, which was then extracted with ethyl acetate (50 mL). The organic layer was washed with water, then, dried over anhydrous magnesium sulfate, and the solvent was evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3), and the title compound (0.44 g, 2.80 mmol, 28%) was obtained as a colorless oil.

1. additionwas added dropwise
2. stirringAfter stirring for 1 hour at 60° C.
3. customwas allowed to room temperature
4. stirringthe solution was further stirred for 30 minutes at room temperature
5. extractionwas then extracted with ethyl acetate (50 mL)
6. washThe organic layer was washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was evaporated in vacuo
9. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3)