反应详情

A solution of tert-butyl (4-(5-(2-amino-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-4-methyl-6-oxo-5,6-dihydropyridin-1(2H)-yl)phenyl)carbamate (112 mg, 0.334 mmol) in a 1:1 mixture of MeOH/THF (˜10 mL) was treated dropwise with CF3COOH and the reaction was allowed to stir for 4 h. One the reaction was completed, the residual CF3COOH was neutralized with NaHCO3 (aq). The reaction was then extracted with EtOAc (3ט10 mL) and brine (˜10 mL). The combined organic layers were dried over anhydrous Na2SO4 (s), filtered and the concentrated in vacuo. The crude organic oil was then purified via column chromatography (MeOH/CHCl3 gradient). Following concentration of the appropriate fractions the title compound was isolated (112 mg, 88%). 1H NMR (DMSO) δ: 7.91 (s, 1H), 7.80(m, 1H), 7.41-7.52 (m, 2H), 7.41 (m, 1H), 7.26-7.32 (m, 2H), 6.65(m, 1H), 6.23 (s, 2H), 6.14 (m, 1H), 4.00 (br. s, H), 3.24 (s, 2H), 2.67 (t, J=5.3 Hz, 2H), 2.34 (s, 3H), 2.22 (s, 3H).

1. extractionThe reaction was then extracted with EtOAc (3ט10 mL) and brine (˜10 mL)
2. dry with materialThe combined organic layers were dried over anhydrous Na2SO4 (s)
3. filtrationfiltered
4. concentrationthe concentrated in vacuo
5. customThe crude organic oil was then purified via column chromatography (MeOH/CHCl3 gradient)
6. customwas isolated (112 mg, 88%)