تفاعل #161011

ord-fd52f1e069014c849097c55dcb05aa8d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated
  2. 2
    درجة الحرارةunder reflux for 2 hours
  3. 3
    غسيلto wash it
  4. 4
    استخلاصthe mixture was extracted with ethyl acetate
  5. 5
    غسيلAfter the obtained organic layer was washed with saturated brine, it
  6. 6
    تجفيفwas dried with anhydrous sodium sulfate
  7. 7
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

الإجراء التجريبي

600 ml of 1N aqueous sodium hydroxide solution was added to a solution of 7.62 g (20 mmol) of 1-[[(4-phenylmethyl-1-piperazinyl)carbonyl]amino]cyclohexanecarboxylic acid ethyl ester in 300 ml of ethanol, and the mixture was heated under reflux for 2 hours. After ether was added to the reaction solution to wash it, the aqueous layer was neutralized by concentrated hydrochloric acid, and the mixture was extracted with ethyl acetate. After the obtained organic layer was washed with saturated brine, it was dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 2.90 g (42%) of the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08829209B2uspto-grants-2014_09