反应详情

N,N-dimethyl-4-pyridinamine (0.01062 mol) and intermediate 5a (0.00708 mol) were suspended in CH2Cl2 (50 ml). A solution of methanesulfonylchloride (0.01062 mol) in CH2Cl2 (30 ml) was added dropwise at room temperature. The mixture was stirred at room temperature for the weekend. N,N-dimethyl-4-pyridinamine (0.00352 mol) and methanesulfonylchloride (0.00358 mol) were added again. The mixture was stirred overnight, washed with water (2×100 ml), dried, filtered over decalite and the solvent was evaporated. The residue was dissolved in MIK (150 ml). Activated charcoal (0.5 g) was added. The mixture was boiled, filtered warm and stirred for 2 hours. The precipitate was filtered off and dried, yielding 1.7 g (50%) of [S-(R*,S*)]-2,4-dihydro-2-(2-methanesulfonyloxy-1-methylpropyl)-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (interm. 5d).

1. stirringThe mixture was stirred overnight
2. washwashed with water (2×100 ml)
3. customdried
4. filtrationfiltered over decalite
5. customthe solvent was evaporated
6. dissolutionThe residue was dissolved in MIK (150 ml)
7. additionActivated charcoal (0.5 g) was added
8. filtrationfiltered
9. temperaturewarm
10. stirringstirred for 2 hours
11. filtrationThe precipitate was filtered off
12. customdried