反应详情

温度

0 °C

To a well-stirred solution of solketal (21, 62.6 ml, 500 mmol), Et3N (83.6 ml, 600 mmol) and DMAP (5 g, 40.9 mmol) in tert-butyl methyl ether (11) at 0° C., n-butyryl chloride (52.4 mL, 500 mmol) was added dropwise over a 75 minute period. The mixture was stirred for an additional hour at 0° C. and then at room temperature for an additional 5 hours. The mixture was diluted with AcOEt (11), washed with water (11), dried (MgSO4), filtered and evaporated to afford 22 (104.6 g, 500 mmol, 100%) as an oil. The material was used in the next step without any further purification.

1. washwashed with water (11)
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. customevaporated