تفاعل #4559

ord-fd27dcb7b04c492084da2155de44a546

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with ether
  2. 2
    غسيلThe combined ether extracts were washed with water
  3. 3
    تجفيفdried over MgSO4
  4. 4
    أخرىthe solvent was removed by rotary evaporation
  5. 5
    أخرىThe residue was purified by HPLC
  6. 6
    غسيلeluting with 95:5 hexane

الإجراء التجريبي

To a solution of 30 ml of 35% HClO4 and 15 ml CH2Cl2 at 0° C. was added 3.0 g (7.55 mmol) 4-(4-(4-bromo-2-fluorophenoxy)phenoxy)-3-methoxy-2-penten-1-ol in 15 ml CH2Cl2. The mixture was stirred at 0° C. for 45 min, then poured into water and extracted with ether. The combined ether extracts were washed with water, dried over MgSO4 and the solvent was removed by rotary evaporation. The residue was purified by HPLC, eluting with 95:5 hexane:acetone, to give 1.9 g (69%) of the product as a clear, colorless oil. Structure was established on the basis of IR and NMR analysis. Calc: C, 55.91; H, 3.86. Found: C, 56.84, H, 4.00.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725683uspto-grants-1988_02