تفاعل #357947

معادلة التفاعل

Bis(2-chloroethyl) amine hydrochloride

3,4-Difluoro-aniline

sodium carbonate

→

1-(3,4-Difluoro-phenyl)-piperazine

المذيبات

nBuOH

n-butanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe nBuOH was evaporated in vacuo
2. 2
   استخلاصthe residue was extracted with ethyl acetate
3. 3
   تجفيفDrying of the organic layer with Na2SO4
4. 4
   تركيزfollowed by concentration
5. 5
   أخرىafforded the crude product
6. 6
   أخرىPurification

الإجراء التجريبي

3,4-Difluoro-aniline (1 g, 7.7 mmol) was dissolved in dry n-butanol (10 mL) and dry sodium carbonate (3.2 g, 30 mmol) was added to it and the reaction mixture stirred for 1 hour under nitrogen. Bis(2-chloroethyl) amine hydrochloride (1.38 g, 7.7 mmol) in nBuOH (10 mL) were then added to the mixture via a syringe. The reaction was then heated at 120° C. for 48 h. The nBuOH was evaporated in vacuo and the residue was extracted with ethyl acetate. Drying of the organic layer with Na2SO4 followed by concentration afforded the crude product. Purification using flash column chromatography (chloroform/methanol) afforded 1-(3,4-Difluoro-phenyl)-piperazine as an off white solid.

المصدر