反应详情

温度

60 °C

To a solution of the product from Step A (1.1 g, 6.7 mmol) in DMF (10 ml) was added sodium hydride (60% in oil, 0.41 g, 10.2 mmol) at room temperature. After stirring for 30 min, chloroacetone (0.79 ml, 10.2 mmol) was added, and the solution heated at 60° C. for 6 h. The reaction mixture was diluted with a saturated aqueous solution of ammonium chloride (10 ml) and extracted with ethyl acetate (3×65 ml). The combined extracts were washed with brine (10 ml), dried (MgSO4), and evaporated to give a residue which was purified by chromatography (silica, 20% to 30% ethyl acetate in hexane) to give an oil (1.3 g, 88%): MS (ES) m/z 219 (M+).

1. extractionextracted with ethyl acetate (3×65 ml)
2. washThe combined extracts were washed with brine (10 ml)
3. dry with materialdried (MgSO4)
4. customevaporated
5. customto give a residue which
6. customwas purified by chromatography (silica, 20% to 30% ethyl acetate in hexane)