海萝胶 → 2,3-二氟对苯二酚

HRID 6333

反应方程式

HRID 6333 反应方程式
[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]

参与物

7

反应物 4

HCID 313海萝胶2 次HCID 24437无水亚硫酸钠HCID 808792,3-二氟苯酚HCID 5462222钾

产物 1

HCID 110299702,3-二氟对苯二酚

试剂、催化剂与溶剂 2

HCID 1140甲苯溶剂HCID 14798二甲基对苯二胺二盐酸溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-32048f4b38654a34b265cba539771b47
来源数据集
uspto-grants-1993_09
专利号
US05248447

关联笔记

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