تفاعل #54735

ord-27b731b27ea44fdfacc7ad82e600c1a0

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةdropwise under cooling
  2. 2
    أخرىreacted at room temperature for 2 hours
  3. 3
    أخرىthe crystals produced
  4. 4
    أخرىwere removed by filtration
  5. 5
    workup.DISTILLATIONThe filtrate was freed of solvent by distillation
  6. 6
    أخرىto leave a residue
  7. 7
    استخلاصThe resulting mixture was extracted with ether
  8. 8
    workup.DISTILLATIONfreed of solvent by distillation
  9. 9
    أخرىto give an oily residue
  10. 10
    workup.DISTILLATIONThis residue was then distilled in vacuo

الإجراء التجريبي

To a solution of 5.4 g of 2-(4-isobutylphenyl)propionic acid chloride and 3.5 g of p-methylbenzyl alcohol in 30 ml of tetrahydrofuran was added 3.7 g of trimethylamine, dropwise under cooling, and reacted at room temperature for 2 hours. After the reaction was complete, the crystals produced were removed by filtration. The filtrate was freed of solvent by distillation to leave a residue, to which was added water. The resulting mixture was extracted with ether, and the extract was dehydrated and freed of solvent by distillation to give an oily residue. This residue was then distilled in vacuo to yield 6.3 g of 2-(4-isobutylphenyl)propionic acid-p-methylbenzyl ester as a colorless oil, boiling at 139°-140° C./0.1 mmHg. Mass spectrum: parent ion 310 m/e.

المصدر

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