تفاعل #54734

ord-e9f0690edfb64c1b8140ef79b651e53a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةdropwise under cooling
  2. 2
    أخرىthe mixture was reacted at room temperature for 1.5 hours
  3. 3
    أخرىthe crystals procuced were removed by filtration
  4. 4
    workup.DISTILLATIONThe filtrate was freed of solvent by distillation
  5. 5
    أخرىto leave a residue
  6. 6
    استخلاصThe resulting mixture was extracted with ether
  7. 7
    استخلاصThe ether extract
  8. 8
    workup.DISTILLATIONfreed of ether by distillation
  9. 9
    أخرىThe oily residue thus obtained
  10. 10
    workup.DISTILLATIONwas distilled in vacuo

الإجراء التجريبي

To a solution of 5.4 g of 2-(4-isobutylphenyl)propionic acid chloride and 3.7 g of m-fluorobenzyl alcohol in 30 ml of tetrahydrofuran was added 3.7 g of triethylamine, dropwise under cooling, and the mixture was reacted at room temperature for 1.5 hours. After the reaction was complete, the crystals procuced 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. The ether extract was dehydrated and freed of ether by distillation. The oily residue thus obtained was distilled in vacuo to yield 5.9 g of 2-(4-isobutylphenyl)propionic acid-m-fluorobenzyl ester as a colorless oil, boiling at 143°-144° C./0.2 mmHg. Mass spectrum: parent ion 314 m/e.

المصدر

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