반응 #69574

반응 방정식

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

DIPEA

HCl

4-(trifluoromethyl)benzenesulfonyl chloride

→

title compound

수율 110.8%

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

수율 110.8%

용매

DCM

DCM

반응 조건

후처리

1. 1
   기타The layers were separated
2. 2
   추출the aqueous layer was then re-extracted with DCM (75 ml)
3. 3
   세척washed with saturated brine solution (100 ml)
4. 4
   기타The organic layers were then separated
5. 5
   건조dried (MgSO4)
6. 6
   농축concentrated to dryness

실험 절차

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).

출처