Nitric Acid → 4,5-Difluoro-2-nitrophenol

HRID 965896ノート

反応式

HRID 965896 の反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[F:8].[N+:10]([O-])([OH:12])=[O:11]>C(O)(=O)C>[F:8][C:7]1[C:2]([F:1])=[CH:3][C:4]([OH:9])=[C:5]([N+:10]([O-:12])=[O:11])[CH:6]=1

参加物

4

反応物 2

HCID 944Nitric AcidHCID 759273,4-Difluorophenol

生成物 1

HCID 27741824,5-Difluoro-2-nitrophenol収率 50%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

In a flask was dissolved 3,4-Difluorophenol (3.10 g, 23.7 mmole) in acetic acid (15 ml). To the stirred solution was added dropwise a solution of fuming HNO3 (1.25 g, 29.7 mmole) in acetic acid (6 ml). The temperature was kept under 50° C. during the entire addition. After completed addition, the mixture was stirred for another hour. The reaction mixture was then poured onto ice-water, giving precipitation of a yellowish solid. The solid was collected by filtration, and dried. The solid was purified on silica (Heptane:EtOAc 5:1), giving the sub-title compound (2.05 g, 50%) as a yellow oil, which crystallizes on standing.

後処理

  1. additionThe temperature was kept under 50° C. during the entire addition
  2. additionaddition
  3. additionThe reaction mixture was then poured onto ice-water
  4. customgiving
  5. customprecipitation of a yellowish solid
  6. filtrationThe solid was collected by filtration
  7. customdried
  8. customThe solid was purified on silica (Heptane:EtOAc 5:1)

出典と根拠

ORDレコード
ord-c782a5d2973642bea38e7d856f2443b7
出典データセット
uspto-grants-2005_10
特許番号
US06951874B2

反応ノート

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