反应详情

Tert-butyl 2-chloropyrimidine-4-carboxylate (4.12 g, 19.2 mmol) and (R)-1-benzyl-3-methylpiperazine (1.83 g, 9.6 mmol) were suspended in acetonitrile (50 ml), followed by addition of N,N-diisopropylethylamine (3.34 ml, 19.2 mmol), and then the resulting liquid was heated at reflux under nitrogen stream for 15 hours. The resulting reaction liquid was concentrated, followed by addition of distilled water (50 ml), and then extracted with MC (100 ml×2). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (1% MeOH/MC), to obtain 3.34 g of yellow solid (94%).

1. temperaturethe resulting liquid was heated
2. temperatureat reflux under nitrogen stream for 15 hours
3. customThe resulting reaction liquid
4. concentrationwas concentrated
5. additionfollowed by addition of distilled water (50 ml)
6. extractionextracted with MC (100 ml×2)
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. filtrationfollowed by filtration and concentration
9. customthe residue thus obtained