反应详情

To a solution of potassium bis(trimethylsilyl)amide (1.13 g, 5.66 mmol) in tetrahydrofuran (10 mL) at 0° C. was added diethyl phosphite (0.73 g, 5.66 mmol). After 10 min, 3-(benzyloxycarbonylamino)propanal (0.78 g, 3.77 mmol) was added as a solution in tetrahydrofuran (5 mL). After 30 min, the reaction was quenched by the addition of 2N hydrochloric acid (25 mL) and extracted with ethyl acetate (50 mL). The organic layer was washed with sat'd sodium chloride (50 mL), dried over magnesium sulfate and concentrated in vacuo. Silica gel chromatography eluting with hexane/acetone (1:1) gave a colorless oil (0.36 g): ESI-MS 346.1 (M+H).

1. waitAfter 30 min
2. customthe reaction was quenched by the addition of 2N hydrochloric acid (25 mL)
3. extractionextracted with ethyl acetate (50 mL)
4. washThe organic layer was washed with sat'd sodium chloride (50 mL)
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. washSilica gel chromatography eluting with hexane/acetone (1:1)