反应详情

A suspension of sodium dimethyl phosphate (14.8 g, 0.1 mmol, from trimethyl phosphate and sodium iodide and acetyl chloride (7.8 g, 0.1 mmol) in dry tetrahydrofuran (80 mn) was stirred for two days at room temperature in a flask fitted with a drying tube. The reaction solution was filtered and the tetrahydrofuran was removed under reduced pressure. The resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr) to give 14.2 g (80%) of dimethyl acetyl phosphate.

1. customfitted with a drying tube
2. filtrationThe reaction solution was filtered
3. customthe tetrahydrofuran was removed under reduced pressure
4. distillationThe resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr)