反应详情

D-Met-OH (1.4 g, 10 mM) and sodium bicarbonate (1.68 g, 20 mM) were added to a mixture of water (15 ml) and DMF (5 ml). Boc-Leu-OSu (3.28 g, 10 mM) in DMF (30 ml) was added thereto and the mixture was stirred overnight at room temperature. After cooling to 0° C., the pH was adjusted to pH 6.5 with 1 N-HCl and the solution was concentrated in vacuo. The residue was dissolved in ethyl acetate-1 N-HCl (50 ml-50 ml). The ethyl acetate layer was washed with water, dried by adding sodium sulfate and ethyl acetate was distilled off. The residue was charged on a column of silica gel (100 g) and eluted with benzene-ethyl acetate (1:1) to obtain Boc-Leu-D-Met-OH (1.6 g).

1. temperatureAfter cooling to 0° C.
2. concentrationthe solution was concentrated in vacuo
3. dissolutionThe residue was dissolved in ethyl acetate-1 N-HCl (50 ml-50 ml)
4. washThe ethyl acetate layer was washed with water
5. customdried
6. additionby adding sodium sulfate and ethyl acetate
7. distillationwas distilled off
8. additionThe residue was charged on a column of silica gel (100 g)
9. washeluted with benzene-ethyl acetate (1:1)