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温度

0 °C

BOC-Ala-OH (94.6 g.), H-Gly-OBzl.TosOH (168.8 g.) and HOBT (67.6 g.) were dissolved in THF (450 ml.) and WSC (91.5 ml.) was added thereto, then stirred for 1 hour at 0° C. and overnight at room temperature. The reaction mixture was concentrated in vacuo and the residue was dissolved in ethyl acetate (800 ml.). 1 N HCl (500 ml.) was added, the precipitate was removed by filtration, and the ethyl acetate layer was washed with 1 N HCl (400 ml.), and twice with 5% sodium bicarbonate solution and water in this order, and, after drying with anhydrous magnesium sulfate, concentrated in vacuo. The residue was treated with n-hexane to obtain crude material (152.5 g.) Recrystallization was carried out twice by ethyl acetate - n-hexane to obtain BOC-Ala-Gly-OBzl (144 g., Yield: 85.7%, m.p.: 87° - 88.5° C., TLC: one spot, RF1 = 0.59).

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in ethyl acetate (800 ml.)
3. addition1 N HCl (500 ml.) was added
4. customthe precipitate was removed by filtration
5. washthe ethyl acetate layer was washed with 1 N HCl (400 ml.)
6. dry with materialtwice with 5% sodium bicarbonate solution and water in this order, and, after drying with anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. additionThe residue was treated with n-hexane
9. customto obtain
10. customcrude material (152.5 g.) Recrystallization