تفاعل #214192

ord-7471a38af4d04b908ade7478567a3151

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 solution of 1.4 g of ethyl 2-[4-(2-oxo-1-cyclopentylidenemethyl)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 afford 0.3 g of the desired product having a boiling point of 210°-215° C./0.2 mmHg (bath temp.). This product solidified and crystallized after cooling. m.p. 106°-107° C.

المصدر

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