반응 #6236

ord-9078b706d8484760a405cf9de643eb4b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과insoluble materials were filtered off
  2. 2
    workup.DISTILLATIONThe volatile component in the filtrate was distilled off
  3. 3
    workup.ADDITIONchloroform was added to the residue
  4. 4
    세척The mixture was washed with brine
  5. 5
    건조dried over potassium carbonate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off

실험 절차

Hydrazine monohydrate [2.99 ml (61.6 mmol)] was added to a suspension of 5.80 g (20.5 mol) of 4-(3-phthalimidopropyloxy)pyridine in 50 ml of ethanol, and the mixture was stirred at room temperature for 3 hours. 100 ml of ethyl acetate was added and insoluble materials were filtered off. The volatile component in the filtrate was distilled off and then chloroform was added to the residue. The mixture was washed with brine and dried over potassium carbonate. The solvent was distilled off to obtain 2.99 g of the desired compound (yield: 99.5%, pale yellow oil).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246948uspto-grants-1993_09