Реакция #69574

Уравнение реакции

1,1-dimethylethyl (3R)-3-methyl-1-piperazinecarboxylate

DIPEA

HCl

4-(trifluoromethyl)benzenesulfonyl chloride

→

title compound

Выход 110.8%

1,1-Dimethylethyl (3R)-3-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinecarboxylate

Выход 110.8%

Растворители

DCM

DCM

Условия реакции

Обработка

1. 1
   ДругоеThe layers were separated
2. 2
   Экстракцияthe aqueous layer was then re-extracted with DCM (75 ml)
3. 3
   Промывкаwashed with saturated brine solution (100 ml)
4. 4
   ДругоеThe organic layers were then separated
5. 5
   Сушкаdried (MgSO4)
6. 6
   Концентрированиеconcentrated to dryness

Методика

To a solution of 1,1-dimethylethyl (3R)-3-methyl-1-piperazinecarboxylate (1.5 g, 7.49 mmol, supplier Aldrich) in DCM (30 ml) was added DIPEA (1.962 ml, 11.23 mmol) and then portionwise addition of 4-(trifluoromethyl)benzenesulfonyl chloride (2.2 g, 8.99 mmol) at room temperature. The resultant mixture was stirred under an atmosphere of Ar for 2 hours before addition of 1M HCl solution (75 ml) and DCM (75 ml). The layers were separated and the aqueous layer was then re-extracted with DCM (75 ml), the organic layers were combined and washed with saturated brine solution (100 ml). The organic layers were then separated, dried (MgSO4) and concentrated to dryness giving the title compound (3.39 g).

Источник