Hydrochloric Acid → 2,3-Difluorobenzene-1,4-diol

HRID 6333

반응식

HRID 6333 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].[K].Cl.S([O-])([O-])=[O:13].[Na+].[Na+]>[OH-].[Na+].C1(C)C=CC=CC=1>[F:1][C:2]1[C:7]([F:8])=[C:6]([OH:13])[CH:5]=[CH:4][C:3]=1[OH:9]

참가 물질

7

반응물 4

HCID 313Hydrochloric Acid2회HCID 24437Sodium SulfiteHCID 808792,3-DifluorophenolHCID 5462222Potassium

생성물 1

HCID 110299702,3-Difluorobenzene-1,4-diol

시약·촉매·용매 2

HCID 1140Toluene용매HCID 14798Sodium Hydroxide용매

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.

후처리

  1. additionDuring this addition
  2. extractionis extracted with ether
  3. temperaturerefluxed for 20 minutes
  4. temperatureAfter cooling
  5. customthe toluene layer is separated off
  6. extractionthe aqueous phase is extracted with ether in a perforator

출처 및 근거

ORD 기록
ord-32048f4b38654a34b265cba539771b47
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248447

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