反应详情

To a solution of tert-butyl 2-(7-(4-chlorobenzyl)-3-methyl-2,6-dioxo-8-(3-(trifluoromethoxy)phenoxy)-2,3,6,7-tetrahydro-1H-purin-1-yl)acetate (200 mg, 0.342 mmol) in DCM (5 ml) was added trifluoroacetic acid (2 ml, 26.9 mmol) at 0° C. The mixture was stirred at 0° C. to room temperature for 3 h. Then the mixture was concentrated, diluted with DCM and water. The phases were separated and the organic phase was washed with brine, dried over sodium sulfate, filtered and concentrated to give 2-(7-(4-chlorobenzyl)-3-methyl-2,6-dioxo-8-(3-(trifluoromethoxy)phenoxy)-2,3,6,7-tetrahydro-1H-purin-1-yl)acetic acid (180 mg, 99.9% yield) as white solid. 1H-NMR (DMSO-d6) δ 13.06(s, 1H), 7.64-7.59(t, 1H), 7.55(s, 1H), 7.48-7.43(m, 5H), 7.36-7.34(d, 1H), 5.43(s, 2H), 4.53(s, 2H), 3.37(s, 3H). LCMS retention time 2.994 min; LCMS MH+ 525.

1. concentrationThen the mixture was concentrated
2. additiondiluted with DCM and water
3. customThe phases were separated
4. washthe organic phase was washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated