sodium dimethyl phosphate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3.00 g (17.75 mmol) of 1,3-dimethyl-2,2-dichloroimidazolidine and 2.63 g (17.77 mmol) of sodium dimethylphosphate are mixed with 20 ml of acetonitrile and 2 ml of water. The reaction mixture is stirred for 12 hours at room temperature, and the precipitate NaCl is subsequently filtered off. The solvent is distilled off, and the residue is dried for 6 hours under a reduced pressure of 7 Pa and at an oil-bath temperature of 70-80° C., giving 4.39 g of 1,3-dimethyl-2-chloroimidazolidinium dimethylphosphate, corresponding to a yield of 95.6%. the precipitate NaCl is subsequently filtered off The solvent is distilled off the residue is dried for 6 hours under a reduced pressure of 7 Pa and at an oil-bath temperature of 70-80° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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. fitted with a drying tube The reaction solution was filtered the tetrahydrofuran was removed under reduced pressure The resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr)