反应详情

2-(t-butyloxycarbonyl)-5-(5-fluoro-4-methylthio-2-pyrimidinyl)-(1S,4S)-2,5-diazabicyclo[2.2.1]heptane (4.50 g, 22.73 mmol), 2-chloro-5-fluoro-4-methylthiopyrimidine [4.64 g (87.5% pure), 22.73 mmol], micropulverized K2CO3 (9.40 g, 68.19 mmol), and KI (0.57 g, 3.41 mmol) in 65 mL of MeCN was refluxed for 44 h. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in a minimum amount of H2O. The solution was extracted with CH2Cl2, washed with saturated NaCl solution, dried over K2CO3, filtered and concentrated under reduced pressured. Flash chromatography (Hexane:EtOAc; 4:1) gave the title compound (6.60 g, 85.4%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutionthe residue was dissolved in a minimum amount of H2O
3. extractionThe solution was extracted with CH2Cl2
4. washwashed with saturated NaCl solution
5. dry with materialdried over K2CO3
6. filtrationfiltered
7. concentrationconcentrated under reduced pressured