Sulfuric Acid → HCID 21429342、化合物

HRID 437608

反応式

HRID 437608 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[OH-].[Na+].[I-].[K+].[I:16]([O-])(=O)=O.[K+].S(=O)(=O)(O)O.S([O-])([O-])=O.[Na+].[Na+]>O.C(O)C>[F:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([OH:8])=[C:6]([I:16])[CH:7]=1

参加物

9

反応物 6

HCID 1118Sulfuric AcidHCID 4875Potassium IodideHCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 1362364-Fluoro-2-nitrophenolHCID 23665710Potassium Iodate

生成物 1

HCID 21429342HCID 21429342、化合物収率 176.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

A slurry of 4-fluoro-2-nitrophenol (3.3 g), sodium hydroxide (0.83 g), potassium iodide (2.33 g) and potassium iodate (1.5 g) in water (21 ml) was added to a stirred mixture of ethanol (16 ml), water (3.5 ml) and concentrated sulphuric acid (1.7 ml) at 50°. The mixture was heated under reflux for 2 hours and was then allowed to stand at room temperature overnight. A small quantity of sodium sulphite was added to decolourise the product and the yellow solid was filtered and crystallised from aqueous ethanol to give yellow crystalls of 4-fluoro-2-iodo-6-nitrophenol (3.5 g) m.p. 40°.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. filtrationthe yellow solid was filtered
  4. customcrystallised from aqueous ethanol

出典と根拠

ORDレコード
ord-e92430831f114d0f9fc0f4e6d18081f9
出典データセット
uspto-grants-1977_06
特許番号
US04031249

関連ノート

読み込み中…