反应详情

(S)-3-[6-(6-Methoxy-5-methyl-pyridin-3-yl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-4-yloxy]-pyrrolidine-1-carboxylic acid tert-butyl ester (2.05 g, 4.63 mmol) was dissolved in TFA/CH2Cl2 (1/2) and stirred at rt for 1 h. The reaction mixture was concentrated under vacuum, the residue was diluted with CH2Cl2, the organic layer washed with NaOH 1N then brine, dried over Na2SO4, filtered and evaporated to give 6-(6-methoxy-5-methyl-pyridin-3-yl)-4-((S)-pyrrolidin-3-yloxy)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidine. 1H NMR (400 MHz, CDCl3, 298K) δ ppm 2.20-2.30 (m, 2 H), 2.22 (s, 3 H), 3.00-3.06 (t, 2 H), 3.09-3.18 (m, 1 H), 3.22-3.37 (m, 3 H), 3.45-3.50 (t, 2 H), 3.95 (s 3 H), 4.10 (s, 2 H), 4.20-4.65 (br.s 1 H), 5.63-5.69 (m, 1 H), 7.21-7.252 (m, 1 H), 7.70-7.74 (m, 1 H), 8.60 (s, 1 H). LCMS: [M+H]+=341.9, Rt(7)=0.61 min.

1. concentrationThe reaction mixture was concentrated under vacuum
2. additionthe residue was diluted with CH2Cl2
3. washthe organic layer washed with NaOH 1N
4. dry with materialbrine, dried over Na2SO4
5. filtrationfiltered
6. customevaporated