تفاعل #505462

معادلة التفاعل

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

المذيبات

DCM

DCM

ظروف التفاعل

المعالجة

1. 1
   أخرىthe layers were separated
2. 2
   غسيلthe organic layer was then washed with 2M NaOH solution (75 ml)
3. 3
   أخرىthe organic layers were separated
4. 4
   تجفيفdried (MgSO4)
5. 5
   تركيزconcentrated to dryness

الإجراء التجريبي

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.

المصدر