反应详情

To a solution of phenylphosphinic acid (5.00 g, 35.2 mmol), anhydrous methanol (7.0 mL, 170 mmol) and 4-dimethylaminopyridine (425 mg, 3.48 mmol) in 50 mL of THF (distilled from ketyl) was added EDAC (8.05 g, 42 mmol) at room temperature. The reaction was stirred for 24 hours then partitioned between HCl solution (75 mL of 1M aq) and ethyl acetate (75 mL). The organic layer was separated, washed with HCl solution (75 mL of 1M aq), sodium bicarbonate solution (75 mL of 5% aq) then dried (sodium sulfate) and concentrated in vacuo to afford the crude title compound as a colorless liquid (1.24 g, 7.95 mmol, 23%).

1. customthen partitioned between HCl solution (75 mL of 1M aq) and ethyl acetate (75 mL)
2. customThe organic layer was separated
3. washwashed with HCl solution (75 mL of 1M aq), sodium bicarbonate solution (75 mL of 5% aq)
4. dry with materialthen dried (sodium sulfate)
5. concentrationconcentrated in vacuo