Sulfuric Acid → 5-Fluoro-2-nitrobenzonitrile

HRID 618678

反応式

HRID 618678 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]#[N:6].[N+:10]([O-])([O-:12])=[O:11].[K+].S(=O)(=O)(O)O>C(Cl)Cl>[F:1][C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[C:4]([CH:3]=1)[C:5]#[N:6]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 678803-Fluorobenzonitrile

生成物 1

HCID 37564675-Fluoro-2-nitrobenzonitrile収率 55.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Fluorobenzonitrile (25 g) was added dropwise to a stirred mixture of potassium nitrate (21.1 g) and concentrated sulphuric acid (150 ml) which had been cooled in a mixture of salt and ice. The mixture was stirred at ambient temperature for 45 minutes. The mixture was poured onto ice (800 ml) and the precipitate was isolated. The solid so obtained was dissolved in methylene chloride, dried (MgSO4) and the solution was evaporated to give 5-fluoro-2-nitrobenzonitrile (19 g).

後処理

  1. temperaturehad been cooled in a mixture of salt and ice
  2. additionThe mixture was poured onto ice (800 ml)
  3. customthe precipitate was isolated
  4. customThe solid so obtained
  5. dry with materialdried (MgSO4)
  6. customthe solution was evaporated

出典と根拠

ORDレコード
ord-cca974b0536343ce985ecaee00ed0664
出典データセット
uspto-grants-1999_09
特許番号
US05955464

関連ノート

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