反应详情

温度

0 °C

(2S)-2-methylpiperazine (15 g, 150 mmol) was dissolved in tetrahydrofuran (300 mL) and the solution was cooled down to 0° C. Sodium hydroxide (150 mL, 449 mmol) was added, then 4-(trifluoromethyl)benzenesulfonyl chloride (40 g, 164 mmol) (dissolved in 200 ml THF) was added dropwise and the resulting mixture was stirred for 1 h. Further 4-(trifluoromethyl)benzenesulfonyl chloride (0.06 eq, 2.2 g) was added and mixture stirred for 10 min. The mixture was diluted with DCM (500 ml) and water (500 ml) and stirred for min. The phases were separated, the aqueous layer was extracted with DCM (1000 ml) and the organic phases concentrated under reduced pressure. The residue was taken-up with 1 M HCl (500 ml) and washed with DCM in order to extracted impurities. The aqueous phase was basified to pH=9 with NaOH 3M, extracted with DCM (3×500 ml) and the combined organic phases dried over Na2SO4 before the solvent was removed under reduced pressure to give the title compound (30 g).

1. stirringmixture stirred for 10 min
2. stirringstirred for min
3. customThe phases were separated
4. extractionthe aqueous layer was extracted with DCM (1000 ml)
5. concentrationthe organic phases concentrated under reduced pressure
6. washwashed with DCM in order
7. extractionto extracted impurities
8. extractionextracted with DCM (3×500 ml)
9. dry with materialthe combined organic phases dried over Na2SO4 before the solvent
10. customwas removed under reduced pressure