反应详情

A solution of tert-butyl 3-(4-((4-(2-(2-amino-2-oxoethyl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)azetidine-1-carboxylate (A82) (0.346 g, 0.623 mmol) and trifluoroacetic acid (1 mL) in DCM (10 mL) was stirred at room temperature for 22 hours. The volatiles were removed in vacuo and 2 M aqueous NaOH (15 mL) was added to the residue. Water (20 mL) was added and the resulting suspension sonicated for 2 minutes, filtered and the filter cake washed with water and dried to give the title compound 20 as a white solid (0.283 g, 99%); 1H NMR (300 MHz, d6-DMSO) δ 10.26 (s, 1H), 8.69 (s, 1H), 7.78 (d, J=8.6 Hz, 2H), 7.43 (s, 1H), 7.36 (d, J=8.6 Hz, 2H), 7.25-7.15 (m, 4H), 6.92 (s, 1H), 4.21 (brs, 2H), 4.06-3.99 (m, 3H), 3.50 (s, 2H), 3.12-3.05 (m, 5H). LCMS-B: rt 5.442 min; m/z 456 [M+H]+.

1. customThe volatiles were removed in vacuo and 2 M aqueous NaOH (15 mL)
2. additionwas added to the residue
3. additionWater (20 mL) was added
4. customthe resulting suspension sonicated for 2 minutes
5. filtrationfiltered
6. washthe filter cake washed with water
7. customdried