反应详情

To a solution of 4-(3-Amino-2-oxopyrrolidine-1-ylmethyl)thiophene-2-carbonitrile hydrochloride (0.43 g, 1.8 mmol), prepared as in EXAMPLE 122, in 10 mL of CH2Cl2 is added 7-methoxynaphthalene-2-sulfonyl chloride (0.51 g, 2 mmol) and triethyl amine (0.55 g, 5.4 mmol). After 16 hours, the solution is diluted with EtOAc and H2O. The layers are separated. The organic layer is washed with 1 N HCl, sat. NaHCO3 and sat. NaCl. The organic layer is dried over MgSO4, filtered and concentrated. The crude product is purified by column chromatography eluting with gradient of 10% EtOAc/CH2Cl2 to 20% EtOAc/CH2Cl2 to afford the title compound (0.50 g, 1.22 mmol) as a white solid.

1. customThe layers are separated
2. washThe organic layer is washed with 1 N HCl, sat. NaHCO3 and sat. NaCl
3. dry with materialThe organic layer is dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product is purified by column chromatography
7. washeluting with gradient of 10% EtOAc/CH2Cl2 to 20% EtOAc/CH2Cl2