반응 #214190

ord-5218d274ac734aa8a9187f0fa2d65feb

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도under reflux for 18 hours
  3. 3
    온도After cooling
  4. 4
    온도cooling
  5. 5
    기타the organic layer was separated
  6. 6
    세척washed with water
  7. 7
    건조After drying over anhydrous sodium sulfate
  8. 8
    workup.DISTILLATIONthe benzene was distilled off
  9. 9
    기타to leave an oily substance
  10. 10
    workup.DISTILLATIONThe substance was distilled under reduced pressure

실험 절차

A mixture of 5.15 g of ethyl 2-(p-formylphenyl)propionate, 4.5 g of pyrrolidinocyclohexene and 20 ml of benzene was heated under reflux for 18 hours. After cooling, the reaction mixture was admixed with a mixture of 5 ml of conc. hydrochloric acid and 5 ml of water under ice-cooling and then stirred at room temperature overnight. 100 ml of benzene were added thereto, the organic layer was separated and then washed with water. After drying over anhydrous sodium sulfate, the benzene was distilled off to leave an oily substance. The substance was distilled under reduced pressure to afford 2.3 g of the desired product as a yellow oily substance having a boiling point of 160°-170° C./0.3 mmHg (bath temp.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04254274uspto-grants-1981_03