反应详情

To a stirred ice-cooled solution of 7-iodo-8-phenyl-2-(2-trimethylsilanyl-ethoxymethyl)-2H-9-oxa-1,2,3a-triaza-cyclopenta[a]naphthalene-3,6-dione (60 mg, 0.112 mmol) in DCM (2 mL) was added TFA (2 mL). The reaction mixture was allowed to warm to RT. After 16 hours, the solvents were removed in vacuo, the residue was dissolved in THF (2 mL) and benzyltrimethylammonium hydroxide (40% in MeOH, 0.05 mL) was added. The reaction mixture was stirred at RT for 1 hour. EtOAc was added and the mixture was washed with water and brine, dried (Na2SO4), filtered, and concentrated in vacuo to give the title compound (50.4 mg) as a buff solid. LCMS (Method B): RT=3.84 min, [M+H]+=406.

1. customthe solvents were removed in vacuo
2. dissolutionthe residue was dissolved in THF (2 mL)
3. additionbenzyltrimethylammonium hydroxide (40% in MeOH, 0.05 mL) was added
4. additionEtOAc was added
5. washthe mixture was washed with water and brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo