Nitric Acid → 2,4-Dihydroxy-5-nitrobenzoic acid

HRID 643930

反応式

HRID 643930 の反応式
[N+:1]([O-:4])(O)=[O:2].[OH:5][C:6]1[CH:14]=[C:13]([OH:15])[CH:12]=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]>CC(O)=O>[OH:5][C:6]1[CH:14]=[C:13]([OH:15])[C:12]([N+:1]([O-:4])=[O:2])=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 14912,4-Dihydroxybenzoic Acid

生成物 1

HCID 166379152,4-Dihydroxy-5-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
0 °C

実験手順

To an ice cold stirred solution of nitric acid (70%, 28 mL) and AcOH (30 mL), is added portionwise 2,4-dihydroxybenzoic acid (7.7 g, 49.9 mmol). The mixture is stirred at 0° C. for 15 min and then slowly warmed to room temperature. The reaction becomes very exothermic and is cooled again in an ice bath to keep the mixture at approximately room temperature. The mixture is stirred at room temperature for 18 h. The resulting precipitate is filtered, washed with water, air dried, then washed with DCM and dried under reduced pressure to afford 2,4-dihydroxy-5-nitrobenzoic acid as a solid: (M−H)−=198.1.

後処理

  1. temperatureslowly warmed to room temperature
  2. temperatureis cooled again in an ice bath
  3. customat approximately room temperature
  4. stirringThe mixture is stirred at room temperature for 18 h
  5. filtrationThe resulting precipitate is filtered
  6. washwashed with water, air
  7. customdried
  8. washwashed with DCM
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-9e199b0885ae48148977de179103fcb5
出典データセット
uspto-grants-2010_04
特許番号
US07700633B2

関連ノート

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