تفاعل #54726

ord-bc15c9be271a4f4ab0bdbd78f546b8e4

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated at 65°-70° C. for 10 hours
  2. 2
    درجة الحرارةthe whole was heated at 95°-100° C. for 8 hours
  3. 3
    استخلاصThe resulting mixture was extracted with ether
  4. 4
    workup.DISTILLATIONthe ether was distilled away from the
  5. 5
    استخلاصextract
  6. 6
    أخرىto leave a residue
  7. 7
    غسيلthe adsorbate was eluted with chloroform

الإجراء التجريبي

A mixture of 0.05 g of sodium and 8 ml of 3-hydroxymethylpyridine was heated at 65°-70° C. for 10 hours. To this mixture was added 3.8 g of 2-(p-isobutylphenyl)propionic acid methyl ester, and the whole was heated at 95°-100° C. for 8 hours. After cooling to room temperature, 100 ml of water was added. The resulting mixture was extracted with ether, and the ether was distilled away from the extract to leave a residue. The residue was passed through a column of silica gel, and the adsorbate was eluted with chloroform. The eluates were freed of chloroform in vacuo to give 2.9 g of 2-(p-isobutylphenyl)propionic acid-3-pyridylmethyl ester as a colorless oil. The infrared spectrum showed strong C=O absorption at 1730 cm-1 characteristic for ester. Mass spectrum: parent ion 297 m/e.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04150137uspto-grants-1979_04