3,4-Dimethylbenzoic acid → 3,4-Dimethyl-5-nitrobenzoic acid

HRID 536430

反応式

HRID 536430 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].[N:12]([O-:14])=[O:13].[K+]>S(=O)(=O)(O)O>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[CH3:11])[C:5]([OH:7])=[O:6]

参加物

4

反応物 2

HCID 120733,4-Dimethylbenzoic acidHCID 516910Potassium nitrite

生成物 1

HCID 113675723,4-Dimethyl-5-nitrobenzoic acid収率 48.1%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

A solution of 3,4-dimethylbenzoic acid (40 g) in concentrated sulphuric acid (250 ml) was cooled to 0° C., treated with a solution of potassium nitrite (27 g) in sulphuric acid (100 ml) dropwise over a period of 1 h, and stirred for 2 h. The reaction mixture was quenched with ice cooled water (100 ml). The solid precipitated was filtered, dissolved in water (2 l), basified with 2N aqueous sodium hydroxide. The solution was acidified to pH 4 with 2N aqueous hydrochloric acid and filtered to get 3,4-dimethyl-5-nitrobenzoic acid (II) (25 g) as colorless solid. The filtrate was further acidified to pH 3 and filtered get 3,4-dimethyl-2-nitrobenzoic acid (I) (13 g) as colorless solid.

後処理

  1. customThe reaction mixture was quenched with ice
  2. temperaturecooled water (100 ml)
  3. customThe solid precipitated
  4. filtrationwas filtered
  5. dissolutiondissolved in water (2 l)
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-c0cac1017daf4671a2aa47d3bf6ad083
出典データセット
uspto-grants-2014_10
特許番号
US08859592B2

関連ノート

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