Reaktion #69574

Reaktionsgleichung

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

DIPEA

HCl

4-(trifluoromethyl)benzenesulfonyl chloride

→

title compound

Ausbeute 110.8%

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

Ausbeute 110.8%

Lösungsmittel

DCM

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe layers were separated
2. 2
   Extraktionthe aqueous layer was then re-extracted with DCM (75 ml)
3. 3
   Waschenwashed with saturated brine solution (100 ml)
4. 4
   SonstigeThe organic layers were then separated
5. 5
   Trocknendried (MgSO4)
6. 6
   Einengenconcentrated to dryness

Vorschrift

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).

Quelle