反应详情

A mixture of compound 3c (320 mg, 0.98 mmol) and LiOH.H2O (123 mg, 2.93 mmol) in THF (8 mL) and H2O (4 mL) was stirred at room temperature for 20 h. The pH of the reaction mixture was adjusted to 5 with aq. 10% HCl. Concentration gave the crude compound 3d. A mixture of compound 3d (0.98 mmol), HOBt (132 mg, 0.98 mmol), Et3N (0.41 mL, 2.93 mmol), EDCI (318 mg, 1.66 mmol), and DMAP (25 mg, 0.21 mmol) in DMF (4 mL) was heated at 65° C. for 5 h. The reaction mixture was cooled to room temperature and diluted with CH2Cl2. The solution was washed with H2O, dried over Na2SO4 and concentrated. Purification by flash column chromatography (silica gel, 3% MeOH/CH2Cl2) gave compound 3e (185 mg).

1. concentrationConcentration
2. customgave the crude compound 3d
3. temperaturewas heated at 65° C. for 5 h
4. temperatureThe reaction mixture was cooled to room temperature
5. washThe solution was washed with H2O
6. dry with materialdried over Na2SO4
7. concentrationconcentrated
8. customPurification by flash column chromatography (silica gel, 3% MeOH/CH2Cl2)