تفاعل #71645

معادلة التفاعل

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

DIPEA

HCl

4-(trifluoromethyl)benzenesulfonyl chloride

→

title compound

المردود 110.8%

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

المردود 110.8%

المذيبات

DCM

DCM

ظروف التفاعل

المعالجة

1. 1
   أخرىThe layers were separated
2. 2
   استخلاصthe aqueous layer was then re-extracted with DCM (75 ml)
3. 3
   غسيلwashed with saturated brine solution (100 ml)
4. 4
   أخرىThe organic layers were then separated
5. 5
   تجفيفdried (MgSO4)
6. 6
   تركيزconcentrated to dryness

الإجراء التجريبي

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).

المصدر