반응 #4559

반응 방정식

4-(4-(4-bromo-2-fluorophenoxy)phenoxy)-3-methoxy-2-penten-1-ol

water

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product

수율 69.0%

4-(4-(4-Bromo-2-fluorophenoxy)phenoxy)-3-oxo-1-pentene

수율 69.0%

용매

CH2Cl2

CH2Cl2

반응 조건

후처리

1. 1
   추출extracted with ether
2. 2
   세척The combined ether extracts were washed with water
3. 3
   건조dried over MgSO4
4. 4
   기타the solvent was removed by rotary evaporation
5. 5
   기타The residue was purified by HPLC
6. 6
   세척eluting with 95:5 hexane

실험 절차

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.

출처