反应详情

温度

70 °C

A mixture of (R)-2-chloro-1-(2-methyloxiran-2-ylmethyl)-4-nitroimidazole prepared in Example 12 (7.00 g, 32.2 mmol) and tert-butyl piperazine-1-carboxylate (6.29 g, 33.8 mmol) and DMF (70 ml) was stirred at 70° C. for 8 hours. The reaction mixture was allowed to return to room temperature, then diluted with water, and then the solution was extracted with ethyl acetate twice. The organic phases were combined, washed with water three times, dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure. To the residue, diethyl ether was added. The precipitates were filtered off, and dried at room temperature under reduced pressure to afford tert-butyl (S)-4-[3-(2-chloro-4-nitroimidazol-1-yl)-2-hydroxy-2-methylpropyl]piperazin-1-carboxylate (10.25 g, yield 79%) as a light yellow powder.

1. customto return to room temperature
2. extractionthe solution was extracted with ethyl acetate twice
3. washwashed with water three times
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure
7. additionTo the residue, diethyl ether was added
8. filtrationThe precipitates were filtered off
9. customdried at room temperature under reduced pressure