Hydroquinone → p-Dihydroxy benzene disulfonic acid

HRID 268233

반응식

HRID 268233 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.O1CCOCC1.[S:15](=[O:19])(=[O:18])([OH:17])O>ClC(Cl)=C(Cl)Cl>[OH:1][C:2]1([S:15]([OH:19])(=[O:18])=[O:17])[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]1[S:15]([OH:17])(=[O:19])=[O:18]

참가 물질

5

반응물 3

HCID 785HydroquinoneHCID 1118Sulfuric AcidHCID 312751,4-Dioxane

생성물 1

HCID 21124945p-Dihydroxy benzene disulfonic acid수율 139%

시약·촉매·용매 1

HCID 31373Tetrachloroethylene용매

반응 조건

온도
140 °C

실험 절차

190 g of p-dihydroxy benzene monosulfonic acid, 100 ml of dioxane, and 100 ml of perchloroethylene are mixed in a flask provided with a reflux condenser. The flask is heated in an oil bath to the reflux temperature (in the oil bath at 140°C). It is refluxed for half an hour, and then is left to cool a little to set the coolant for distillation. In the flask, two layers are formed: a colourless lower layer, and a coloured upper layer in which the acid is dissolved. The flask is heated again and 100 ml of the solvent mixture are distilled. In the mixture collected, two layers form, the upper, moderate, is aqueous. To the flask provided with a reflux condenser, 98 g of sulfuric acid containing 20 % of SO3 are added, and it is heated again, to a lower temperature, so that the reflux is barely noticeable (bath temperature: 130°C), for four hours. The liquids accompanying the acid are removed by distilling at reduced pressure, the residue is dissolved in a little water, 2 g of active charcoal are added, and it is filtered. The solution is concentrated, cooled, and is precipitated by adding five volumes of acetone. The precipate is filtered, and 189 g of p-dihydroxy benzene disulfonic acid, with a melting point of 166° - 169°C are obtained.

후처리

  1. customprovided with a reflux condenser
  2. temperatureIt is refluxed for half an hour
  3. waitis left
  4. temperatureto cool a little
  5. distillationfor distillation
  6. customIn the flask, two layers are formed
  7. dissolutiona colourless lower layer, and a coloured upper layer in which the acid is dissolved
  8. temperatureThe flask is heated again
  9. distillation100 ml of the solvent mixture are distilled
  10. customIn the mixture collected
  11. customTo the flask provided with a reflux condenser
  12. temperatureit is heated again, to a lower temperature, so that the reflux
  13. custom(bath temperature: 130°C)
  14. customare removed
  15. distillationby distilling at reduced pressure
  16. dissolutionthe residue is dissolved in a little water, 2 g of active charcoal
  17. additionare added
  18. filtrationit is filtered
  19. concentrationThe solution is concentrated
  20. temperaturecooled
  21. customis precipitated
  22. additionby adding five volumes of acetone
  23. filtrationThe precipate is filtered

출처 및 근거

ORD 기록
ord-521c9407e4a64a9ca0c93b936b9cd4bd
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947448

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