Water → 5-Chloro-2-hydroxy-3-nitrobenzoic acid

HRID 2271264ノート

反応式

HRID 2271264 の反応式
[OH:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Cl:14]C1C=C(C(O)=O)C(O)=CC=1.O>C(O)(=O)C>[Cl:14][C:8]1[CH:7]=[C:3]([C:4]([OH:6])=[O:5])[C:2]([OH:1])=[C:10]([N+:11]([O-:13])=[O:12])[CH:9]=1

参加物

5

反応物 3

HCID 962Water2 回HCID 68073-Nitrosalicylic acid2 回HCID 94475-Chlorosalicylic Acid

生成物 1

HCID 4120785-Chloro-2-hydroxy-3-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

The following procedure demonstrates the preparation of compound 1 with X=5-Cl, with comparable procedures being useful for obtaining related compounds having different X substituents. A solution suspension of 10 g of 5-chlorosalicylic acid in 50 mL glacial acetic acid was cooled in an ice bath until the solvent began to freeze. The bath was exchanged to a room temperature water bath and 4.47 g of 90% fuming nitric acid (1:1 equivalent) in 3 mL glacial acetic acid was added dropwise. After addition was complete, the mixture was stirred for 150 minutes at room temperature (R.T.) in the water bath. It was then poured into 120 mL of ice and water and stirred in an ice bath for 30 minutes. The precipitated solid was collected by filtration and air-dried overnight.

後処理

  1. customfor obtaining
  2. temperaturewas cooled in an ice bath until the solvent
  3. customwas exchanged to a room temperature
  4. additionAfter addition
  5. filtrationThe precipitated solid was collected by filtration
  6. customair-dried overnight

出典と根拠

ORDレコード
ord-4899cfeda53543bbb55d7e657d429d7c
出典データセット
uspto-grants-2001_12
特許番号
US06333432B1

反応ノート

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