氢溴酸 → 2-氟苯乙基溴

HRID 362836

反应方程式

HRID 362836 反应方程式
[BrH:1].S(=O)(=O)(O)O.[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:14][CH2:15]O>>[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:14][CH2:15][Br:1]

参与物

4

反应物 3

HCID 260氢溴酸HCID 1118四氧化硫HCID 27332962-氟苯乙醇

产物 1

HCID 27569642-氟苯乙基溴收率 99%

实验过程

To a mixture of aqueous hydrobromic acid (48%, 360 mL) and concentrated sulfuric acid (103.6 mL) at room temperature was added dropwise 2-(2-fluorophenyl)ethanol (250 g, 1.78 mol, Aldrich). The reaction mixture was refluxed for 7 h, poured onto 600 ml of ice and the mixture was extracted with diethyl ether. The diethyl ether extracts were washed successively with saturated sodium carbonate and brine. The organic phase was dried (MgSO4) and concentrated in vacuo to give 359.9 g (99%) of 2-(2-fluorophenyl)-ethylbromide as a brown oil. This product was used without further purification. NMR (CDCl3 : d 7.6-6.9 (m. 4H, ArH), 3.6 (t, 2H CH2), 3.2 (t, 2H, CH2).

后处理

  1. temperatureThe reaction mixture was refluxed for 7 h
  2. extractionthe mixture was extracted with diethyl ether
  3. washThe diethyl ether extracts were washed successively with saturated sodium carbonate and brine
  4. dry with materialThe organic phase was dried (MgSO4)
  5. concentrationconcentrated in vacuo

来源与证据

ORD记录
ord-94c84f6978a34477bbb058ea20e1f0a0
来源数据集
uspto-grants-1999_02
专利号
US05872118

关联笔记

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