反应详情

A solution of tert-butyl 7-((3-cyanobenzyl)oxy)-5-oxo-2,3-dihydroimidazo[1,2-c]pyrim-idine-1(5H)-carboxylate (20 mg, 0.054 mmol) in dichloromethane (DCM) (4 mL) was added TFA (0.5 mL, 6.49 mmol) at room temperature. The reaction mixture was stirred at rt overnight, then concentrated to remove solvent, diluted with sat. NaHCO3 (5 mL) solution and EtOAc (15 mL). Separated organic part was dried over Na2SO4, filtered and concentrated. Purification via MDAP (Gilson GX-281, mobile phase: 0.01% NH4HCO3, CH3CN/water, 50˜95%) afforded the title product (9 mg) as a white solid.

1. concentrationconcentrated
2. customto remove solvent
3. additiondiluted with sat. NaHCO3 (5 mL) solution and EtOAc (15 mL)
4. dry with materialSeparated organic part was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification via MDAP (Gilson GX-281, mobile phase: 0.01% NH4HCO3, CH3CN/water, 50˜95%)