반응 #6429

ord-32048f4b38654a34b265cba539771b47

반응 방정식

Cl
hydrochloric acid
Cl
hydrochloric acid
O=S([O-])[O-].[Na+].[Na+]
sodium sulphite
[K]
potassium
Oc1cccc(F)c1F
2,3-difluorophenol
Oc1ccc(O)c(F)c1F
2,3-difluorohydroquinone

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONDuring this addition
  2. 2
    추출is extracted with ether
  3. 3
    온도refluxed for 20 minutes
  4. 4
    온도After cooling
  5. 5
    기타the toluene layer is separated off
  6. 6
    추출the aqueous phase is extracted with ether in a perforator

실험 절차

1 mol of 2,3-difluorophenol is dissolved in 1 l of 10% sodium hydroxide solution, and a saturated aqueous solution of 1.1 mol of potassium peroxodisulphate is added dropwise over the course of 4 hours with ice cooling. During this addition, the temperature must not exceed 20o The mixture is stirred overnight at room temperature and neutralized using hydrochloric acid, and unreacted starting material is extracted with ether. 3 1 of toluene and 2 mol of sodium sulphite are added to the aqueous phase, and the mixture is strongly acidified using 1 1 of concentrated hydrochloric acid and refluxed for 20 minutes. After cooling, the toluene layer is separated off, the aqueous phase is extracted with ether in a perforator, and 2,3-difluorohydroquinone is obtained by evaporating the combined toluene and ether extracts.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05248447uspto-grants-1993_09