反应详情

In tetrahydrofuran (8 ml), 1-tert-butoxycarbonyl-4-methanesulfonylpiperazine (838 mg) was dissolved, followed by the addition of tert-butyl lithium (a 1.7M pentane solution, 1.72 ml) at −78° C. in an argon gas atmosphere. The resulting mixture was stirred for 2 hours. After the dropwise addition of a solution of 6-chloronicotinaldehyde (346 mg) in tetrahydrofuran (tetrahydrofuran: 4 ml) and stirring at −78° C. for 3 hours, the reaction mixture was added with isopropanol (1 ml). The resulting mixture was heated to room temperature and diluted with ethyl acetate. The diluted solution was washed with water and saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was recrystallized from ethyl acetate, whereby the title compound (532 mg, 54%) was obtained.

1. stirringstirring at −78° C. for 3 hours
2. washThe diluted solution was washed with water and saturated aqueous NaCl solution
3. dry with materialdried over anhydrous sodium sulfate
4. customThe residue obtained
5. distillationby distilling off the solvent under reduced pressure
6. customwas recrystallized from ethyl acetate, whereby the title compound (532 mg, 54%)
7. customwas obtained