تفاعل #2252113

ord-2d13c7216a6b4b9686a238de66c3d21e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux
  2. 2
    درجة الحرارةreflux
  3. 3
    workup.WAITAfter 50 hours
  4. 4
    تركيزAfter a total reflux time of 108 hours, the reaction mixture was concentrated in vacuo
  5. 5
    أخرىthe residue was purified by high pressure liquid chromatography

الإجراء التجريبي

A mixture of 6.0 g of (4-acetyl-3-hydroxy-2-propylphenoxy)acetic acid ethyl ester, 25 ml of bis(2-chloroethyl)ether and 2.2 g of anhydrous potassium carbonate in 150 ml of anhydrous acetone was stirred at reflux. After 24 hours, 2 g of potassium iodide and 50 ml of anhydrous dimethylformamide were added and reflux was continued. After 50 hours, 2.2 g of potassium carbonate and 2 g of potassium iodide were added and after 77 hours, 2.0 g of potassium carbonate was added. After a total reflux time of 108 hours, the reaction mixture was concentrated in vacuo and the residue was purified by high pressure liquid chromatography using 25% ethyl acetate-hexane to give 5.96 g (72% yield) of [4-acetyl-3-[2-(2-chloroethoxy)ethoxy]-2-propylphenoxy]acetic acid ethyl ester as an oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04507498uspto-grants-1985_03