反应详情

2(S)-(tert-Butoxycarbonylamino)-3-phenylpropionic acid (39.80 g, 0.150 mol), N,O-dimethylhydroxylamine hydrochloride (21.95 g, 0.225 mol), EDC hydrochloride (31.52 g, 0.165 mol) and HOBT (20.25 g, 0.150 mol) were stirred in dry, degassed DMF (200 mL) at 20° C. under nitrogen. N-Methylmorpholine is added to obtain pH 7. The reaction was stirred overnight, the DMF distilled under high vacuum, and the residue partitioned between ethyl acetate and 2% potassium hydrogen sulfate. The organic phase was washed with saturated sodium bicarbonate, water, and saturated brine, and dried with magnesium sulfate. The solvent was removed in vacuo to give the title compound.

1. customin dry
2. customdegassed DMF (200 mL) at 20° C. under nitrogen
3. additionN-Methylmorpholine is added
4. customto obtain pH 7
5. distillationthe DMF distilled under high vacuum
6. customthe residue partitioned between ethyl acetate and 2% potassium hydrogen sulfate
7. washThe organic phase was washed with saturated sodium bicarbonate, water, and saturated brine
8. dry with materialdried with magnesium sulfate
9. customThe solvent was removed in vacuo