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

HRID 4463

반응식

HRID 4463 반응식
[Br:1][C:2]1[CH:23]=[CH:22][C:5]([O:6][C:7]2[CH:21]=[CH:20][C:10]([O:11][CH:12]([CH3:19])[C:13]([O:17]C)=[CH:14][CH2:15]O)=[CH:9][CH:8]=2)=[C:4]([F:24])[CH:3]=1.O>C(Cl)Cl>[Br:1][C:2]1[CH:23]=[CH:22][C:5]([O:6][C:7]2[CH:21]=[CH:20][C:10]([O:11][CH:12]([CH3:19])[C:13](=[O:17])[CH:14]=[CH2:15])=[CH:9][CH:8]=2)=[C:4]([F:24])[CH:3]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 543727674-(4-(4-Bromo-2-fluorophenoxy)phenoxy)-3-methoxy-2-penten-1-ol

생성물 1

HCID 201525974-(4-(4-Bromo-2-fluorophenoxy)phenoxy)-3-oxo-1-pentene수율 69%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

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.

후처리

  1. extractionextracted with ether
  2. washThe combined ether extracts were washed with water
  3. dry with materialdried over MgSO4
  4. customthe solvent was removed by rotary evaporation
  5. customThe residue was purified by HPLC
  6. washeluting with 95:5 hexane

출처 및 근거

ORD 기록
ord-fd27dcb7b04c492084da2155de44a546
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725683

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