反应详情

To an ice-cooled solution of the mixture of [1-(6-fluoro-3,4-dihydro-5-oxa-1,2a-diaza-acenaphthylen-2-yl)ethyl]carbamic acid tert-butyl ester and N-[1-(6-fluoro-3,4-dihydro-5-oxa-1,2a-diaza-acenaphthylen-2-yl)ethyl]acetamide from the previous step in DCM (15 mL) was added TFA (3 mL) and the mixture was stirred at RT for 2 h. Toluene was added and volatiles were removed under reduced pressure, the resulting residue was dissolved in MeOH and loaded onto an Isolute® SCX-2 cartridge. The cartridge was washed with MeOH and the product was eluted with 0.5M NH3/MeOH. The product containing fractions were combined and concentrated in vacuo. Purification by column chromatography (Si—PCC, gradient 2-8% 2M NH3/MeOH in DCM) afforded the title compound as a light brown gum (185.6 mg, 65%, 2 steps). LCMS (Method B): RT 1.54 min [M+H]+ 222

1. customvolatiles were removed under reduced pressure
2. dissolutionthe resulting residue was dissolved in MeOH
3. washThe cartridge was washed with MeOH
4. washthe product was eluted with 0.5M NH3/MeOH
5. additionThe product containing fractions
6. concentrationconcentrated in vacuo
7. customPurification by column chromatography (Si—PCC, gradient 2-8% 2M NH3/MeOH in DCM)