反应详情

温度

50 °C

Mixture of (R)-2-bromo-4-nitro-1-(2-methyl-2-oxiranylmethyl)imidazole (2.04 g) prepared in example 6, 3-(4-trifluoromethylphenyl)-2-propenyl piperazin-1-carboxylate (2.69 g) and N,N-dimethylformamide (10 ml) was stirred at 50° C. for 20 hours. The reaction mixture was turned back to a room temperature, water (45 ml) was added, then extracted twice with ethyl acetate (15 ml). The organic layers were combined together, washed with water 3 times, dried over anhydrous sodium sulfate. Afer being filtrated under a reduced pressure, the residue thus obtained was purified by use of a silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/2), there was obtained 3-(4-trifluoromethylphenyl)-2-propenyl (S)-4-[3-(2-bromo-4-nitroimidazol-1-yl)-2-hydroxy-2-methylpropyl]piperazin-1-carboxylate (3.77 g, yield: 84%)

1. customwas turned back to a room temperature
2. extractionextracted twice with ethyl acetate (15 ml)
3. washwashed with water 3 times
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfer being filtrated under a reduced pressure
6. customthe residue thus obtained
7. customwas purified by use of a silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/2)