反应详情

(R)-tert-butyl 3-methyl-1-oxo-1-(2,2,2-trifluoroethylamino)butan-2-ylcarbamate I-3a (12.81 g, 42.9 mmol) was dissolved in DCM (30 ml), and TFA (12 ml, 156 mmol) slowly added. The reaction was allowed to stir at room temperature for 2 hr. The mixture was concentrated in vacuo to an oil. The oil was dissolved in DCM and washed with aq. sodium bicarbonate (50 mL) dried over sodium sulfate, filtered and concentrated to an oil. The oil was dissolved in ethyl acetate, cooled to 0° C. and treated with 1N HCL in diethyl ethere to give upon filtration 10.0 gm solid.

1. concentrationThe mixture was concentrated in vacuo to an oil
2. dissolutionThe oil was dissolved in DCM
3. washwashed with aq. sodium bicarbonate (50 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to an oil
7. dissolutionThe oil was dissolved in ethyl acetate
8. temperaturecooled to 0° C.
9. additiontreated with 1N HCL in diethyl