반응 #505462

반응 방정식

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

DIPEA

HCl

4-[(trifluoromethyl)oxy]benzenesulfonyl chloride

→

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

용매

DCM

DCM

반응 조건

후처리

1. 1
   기타the layers were separated
2. 2
   세척the organic layer was then washed with 2M NaOH solution (75 ml)
3. 3
   기타the organic layers were separated
4. 4
   건조dried (MgSO4)
5. 5
   농축concentrated to dryness

실험 절차

To a solution of 1,1-dimethylethyl(3R)-3-methyl-1-piperazinecarboxylate (605 mg, 2.56 mmol) in DCM (20 ml) was added DIPEA (1.12 ml, 6.39 mmol) and then portionwise 4-[(trifluoromethyl)oxy]benzenesulfonyl chloride (0.455 ml, 2.68 mmol) at room temp and the resultant mixture stirred under Ar for 16 h. DCM (75 ml) and a 1M HCl solution (75 ml) were added, the layers were separated and the organic layer was then washed with 2M NaOH solution (75 ml), the organic layers were separated, dried (MgSO4) and concentrated to dryness. 1,1-Dimethylethyl(3R)-3-methyl-4-({4-[(trifluoromethyl)oxy]phenyl}sulfonyl)-1-piperazinecarboxylate was isolated as a slowly crystallizing white solid.

출처