反应详情

A mixture of 1-(2-tert-butylphenyl)piperazine dihydrochloride obtained in Reference Example 1 (10.0 g, 34.3 mmol), 4-bromobenzoyl chloride (8.2 g, 37.4 mmol) and triethylamine (16.7 mL, 120.0 mmol) in tetrahydrofuran (200 mL) was stirred at room temperature for 16 h. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to purify the residue by NH-silica gel column chromatography (hexane/ethyl acetate 50:50 to 0:100). Solvent was removed to obtain a solid (14.2 g, quant.).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customto purify the residue by NH-silica gel column chromatography (hexane/ethyl acetate 50:50 to 0:100)
7. customSolvent was removed
8. customto obtain a solid (14.2 g, quant.)