Potassium Nitrate → 2-Chloro-4-fluoro-5-methyl-3-nitrobenzoic acid

HRID 369243ノート

反応式

HRID 369243 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([CH3:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:10]([N+:13]([O-:15])=[O:14])=[C:9]([F:11])[C:8]([CH3:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 23284674Benzoic acid, 2-chloro-4-fluoro-5-methyl-

生成物 1

HCID 232847252-Chloro-4-fluoro-5-methyl-3-nitrobenzoic acid収率 91%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

2-Chloro-4-fluoro-5-methylbenzoic acid (2.0 g) was added to concentrated sulfuric acid (20 ml) to dissolve it, and potassium nitrate (1.07 g) was added portionwise to the solution under ice cooling. After the addition, the temperature of the reaction mixture was given back to room temperature to conduct stirring overnight. The reaction mixture was poured into ice water and extracted with diethyl ether. After an organic layer was collected and dried over anhydrous magnesium sulfate, the solvent was distilled off to obtain the title compound (2.25 g) as a reddish brown oil.

後処理

  1. additionwas added portionwise to the solution under ice cooling
  2. additionAfter the addition
  3. customwas given back to room temperature
  4. extractionextracted with diethyl ether
  5. customAfter an organic layer was collected
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-7734ae73e96846fc8d9d7bda4d119a84
出典データセット
uspto-grants-2000_10
特許番号
US06136823

反応ノート

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