六水硝酸铽 → 3,4-二氟硝基苯

HRID 66103

反应方程式

HRID 66103 反应方程式
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[F:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[F:17]>>[F:10][C:11]1[CH:16]=[C:15]([N+:1]([O-:4])=[O:2])[CH:14]=[CH:13][C:12]=1[F:17]

参与物

4

反应物 3

HCID 944六水硝酸铽HCID 1118四氧化硫HCID 97061,2-二氟苯

产物 1

HCID 1230533,4-二氟硝基苯

反应条件

温度
-12 °C

实验过程

This material is prepared as described by R. W. Taft, G. B. Klingensmith, and S. Ehrenson, (J. Am. Chem. Soc., 87, 3620 (1965)). To a stirred mixture of 5.0 ml of concentrated nitric acid and 13.9 ml of concentrated sulfuric acid cooled to -12° C. is added 9.7 g (0.085 mole) of 1,2-difluorobenzene. A slight exotherm is observed and the mixture is cooled to -20° C. whereupon it solidifies. The mixture is stirred for 45 minutes at -5° to 0° and is then allowed to warm slowly to room temperature. After 1 hour the mixture is poured onto ice, and the mixture extracted with diethyl ether (3×75 ml). The combined ether extracts are washed with water, 10% aqueous Na2CO3, and water again. The ether solution is dried (MgSO4) and concentrated in vacuo without external heating to give the crude product (11.9 g), which is distilled (kugelrohr apparatus) to give 10.2 g of colorless liquid. The nmr spectrum of this material is consistent with the structure.

后处理

  1. customThis material is prepared
  2. temperaturethe mixture is cooled to -20° C. whereupon it
  3. temperatureto warm slowly to room temperature
  4. additionAfter 1 hour the mixture is poured onto ice
  5. extractionthe mixture extracted with diethyl ether (3×75 ml)
  6. washThe combined ether extracts are washed with water, 10% aqueous Na2CO3, and water again
  7. dry with materialThe ether solution is dried (MgSO4)
  8. concentrationconcentrated in vacuo
  9. temperaturewithout external heating
  10. customto give the crude product (11.9 g), which
  11. distillationis distilled (kugelrohr apparatus)

来源与证据

ORD记录
ord-d4a5f129cbac44878fc983b98b2e1f88
来源数据集
uspto-grants-1978_12
专利号
US04130561

关联笔记

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