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

HRID 6333

反応式

HRID 6333 の反応式
[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]

参加物

7

反応物 4

HCID 313Hydrochloric Acid2 回HCID 24437Sodium SulfiteHCID 808792,3-DifluorophenolHCID 5462222Potassium

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32048f4b38654a34b265cba539771b47
出典データセット
uspto-grants-1993_09
特許番号
US05248447

関連ノート

読み込み中…