تفاعل #1989935

ord-b9f8d486d95b4204aa8d44b9ced88b30

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux for 18 hours
  3. 3
    درجة الحرارةAfter cooling
  4. 4
    درجة الحرارةcooling
  5. 5
    أخرىthe organic layer was separated
  6. 6
    غسيلwashed with water
  7. 7
    تجفيفAfter drying over anhydrous sodium sulfate
  8. 8
    workup.DISTILLATIONthe benzene was distilled off
  9. 9
    أخرىto leave an oily substance
  10. 10
    workup.DISTILLATIONThe substance was distilled under reduced pressure

الإجراء التجريبي

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.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04365076uspto-grants-1982_12