Potassium Nitrate → Benzoic acid,2,3,6-trifluoro-5-nitro-

HRID 1638663

反応式

HRID 1638663 の反応式
[F:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]([F:12])[C:3]=1[C:4]([OH:6])=[O:5].[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[F:12][C:7]1[C:8]([N+:13]([O-:15])=[O:14])=[CH:9][C:10]([F:11])=[C:2]([F:1])[C:3]=1[C:4]([OH:6])=[O:5]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 5200622,3,6-Trifluorobenzoic acid

生成物 1

HCID 15631828Benzoic acid,2,3,6-trifluoro-5-nitro-収率 83.4%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

2,3,6-Trifluorobenzoic acid (21.0 g) is added to conc. sulfuric acid (120 ml) under ice-cooling. To the mixture is added dropwise a solution of potassium nitrate (14.5 g) in conc sulfuric acid (30 ml) at below 20° C. After the addition, the mixture is stirred at room temperature for one hour. The reaction mixture is poured into ice water and extracted with diethyl ether. The extract is dried over magnesium sulfate, and then the solvent is distilled off. The residue is recrystallized from dichloromethane-n-hexane to give 2,5,6-trifluoro-3-nitrobenzoic acid (22 g), as colorless prisms, m.p. 98°-99° C.

後処理

  1. temperaturecooling
  2. additionAfter the addition
  3. extractionextracted with diethyl ether
  4. dry with materialThe extract is dried over magnesium sulfate
  5. distillationthe solvent is distilled off
  6. customThe residue is recrystallized from dichloromethane-n-hexane

出典と根拠

ORDレコード
ord-b5254972de5341e0b25ff1d9a8773f6d
出典データセット
uspto-grants-1989_11
特許番号
US04880806

関連ノート

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