反应详情

温度

0 °C

After dissolving 537 mg of 1-(tert-butoxycarbonyl)-4-cyano-4-(hydroxymethyl)piperidine in 100 ml of tetrahydrofuran, 0.4 ml of triethylamine was added and the solution was cooled to 0° C. 0.2 ml of methanesulfonyl chloride was added and the mixture was stirred overnight at room temperature. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. After adding water to the residue, extraction was performed with ethyl acetate. The organic layer was washed with water and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (799 mg, 100% yield).

1. additionwas added
2. filtrationThe reaction mixture was filtered
3. concentrationthe filtrate was concentrated under reduced pressure
4. additionAfter adding water
5. extractionto the residue, extraction
6. washThe organic layer was washed with water
7. dry with materialdried over magnesium sulfate
8. distillationThe solvent was distilled off under reduced pressure