تفاعل #214193

ord-0cd3f510e8604077931ac1f610f5c03e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder reflux for 1 hour
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    استخلاصthe reaction mixture was extracted with ether
  4. 4
    غسيلThe extract was washed with water
  5. 5
    تجفيفdried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONThe ether was distilled off
  7. 7
    أخرىto leave an oily substance, which
  8. 8
    workup.DISTILLATIONvacuum distilled

الإجراء التجريبي

A solutionof 1.3 g of ethyl 2-(4-(2-oxo-1-cyclohexylidenemethyl)phenyl)propionate in 15 ml of dioxane and 100 ml of a 10% aqueous solution of hydrogen bromide was heated under reflux for 1 hour. After cooling, the reaction mixture was extracted with ether. The extract was washed with water and dried over anhydrous sodium sulfate. The ether was distilled off to leave an oily substance, which was then vacuum distilled to give 0.6 g of the desired product having a boiling point of 210°-215° C./0.3 mmHg (bath temp.). This product solidified and crystallized after cooling. m.p. 108°-110° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04254274uspto-grants-1981_03