反应详情

A solution of N-benzyloxycarbonyl-L-proline (5 g, 20.06 mmol), morpholine (1.92 ml, 20.06 mmol), and N-hydroxysuccinimide (2.31 g, 20.06 mmol) in N, N-dimethylformamide (100 ml) was added DCC (4.14 g, 20.06 mmol) and the resulting mixture was stirred for 4 h at room temperature. After the precipitation was filtered off, the filtrate was concentrated in vacuo. The residue was dissolved in ethyl acetate and the resulting precipitation was filtered off. After the filtrate was washed with dilute hydrochloric acid, saturated sodium hydrogencarbonate aq., and water, the organic layer was dried over magnesium sulfate and concentrated in vacuo. The residue was crystallized from the mixed solvents of ethyl acetate-hexane to give the compound (34) (4.44 g, 69.5%).

1. customAfter the precipitation
2. filtrationwas filtered off
3. concentrationthe filtrate was concentrated in vacuo
4. dissolutionThe residue was dissolved in ethyl acetate
5. customthe resulting precipitation
6. filtrationwas filtered off
7. washAfter the filtrate was washed with dilute hydrochloric acid, saturated sodium hydrogencarbonate aq., and water
8. dry with materialthe organic layer was dried over magnesium sulfate
9. concentrationconcentrated in vacuo
10. customThe residue was crystallized from the mixed solvents of ethyl acetate-hexane