反应详情

Two 20 mL microwave vials were each charged with a half portion of 6-benzyl-4-chloro-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (5.62 g, 21.6 mmol), (6-(trifluoromethyl)pyridin-3-yl)methanamine (5.0 g, 28 mmol), N,N-diisopropylethylamine (7.6 mL, 44 mmol) and acetonitrile (10 mL), and the mixture was subjected to a microwave irradiation at 200° C. for 3.5 h. LC-MS analysis showed the reaction was complete for both samples. The samples were combined, and partitioned between CH2Cl2 (150 mL) and 0.5M NaH2PO4 (pH 4; 120 mL). The organic layer was extracted with 2M HCl (60 mL, 30 mL). The combined acid extracts were basified with 50% KOH (25 mL), extracted with CH2Cl2 (2×100 mL), dried (Na2SO4), filtered and concentrated to yield a light brown oil, which was absorbed on silica (40 g) and purified by column (120 g silica gel, 0-7.5% MeOH/CH2Cl2) to afford a light yellow foam (7.42 g, 86%).

1. customthe mixture was subjected to a microwave irradiation at 200° C. for 3.5 h
2. custompartitioned between CH2Cl2 (150 mL) and 0.5M NaH2PO4 (pH 4; 120 mL)
3. extractionThe organic layer was extracted with 2M HCl (60 mL, 30 mL)
4. extractionextracted with CH2Cl2 (2×100 mL)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customto yield a light brown oil, which
9. customwas absorbed on silica (40 g)
10. custompurified by column (120 g silica gel, 0-7.5% MeOH/CH2Cl2)