反应详情

2-Methyl-4,6-dichloropyrimidine (430 mg; 2.64 mMol) was refluxed in p-dioxane 10 mL with DIEA (575 uL; 426 mg; 3.3 mMol) and aniline (239 uL; 247 mg; 2.65 mMol) for 48 hrs under N2. The solvent was removed under reduced pressure and the residue partitioned between ethyl acetate and 0.5 N HCl. The organic fraction was washed with water, brine, and dried over Na2SO4) and the solvent removed under reduced pressure. Crude material was triturated with MTBE, suction filtered to isolate and washed with more MTBE and air dried to afford 375 mg of white solid, 64.5% yield. 1H NMR (500 MHz DMSO-d6) d 8.9 (s, 1H), 7.7 (s, 1H), 7.55 (m, 2H), 7.27 (t, 2H), 6.95 (t, 1H), 6.0 (s, 1H) 2.25 (s, 3H) ppm

1. customThe solvent was removed under reduced pressure
2. customthe residue partitioned between ethyl acetate and 0.5 N HCl
3. washThe organic fraction was washed with water, brine
4. dry with materialdried over Na2SO4) and the solvent
5. customremoved under reduced pressure
6. customCrude material was triturated with MTBE, suction
7. filtrationfiltered
8. customto isolate
9. washwashed with more MTBE and air
10. customdried