3,5-Diaminobenzoic acid → 3,5-Bis(methoxyacetylamino)benzoic acid

HRID 1165881ノート

反応式

HRID 1165881 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([NH2:11])[CH:10]=1)[C:5]([OH:7])=[O:6].[CH3:12][O:13][CH2:14][C:15](Cl)=[O:16]>N1C=CC=CC=1>[CH3:12][O:13][CH2:14][C:15]([NH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([NH:11][C:15](=[O:16])[CH2:14][O:13][CH3:12])[CH:10]=1)[C:5]([OH:7])=[O:6])=[O:16]

参加物

4

反応物 2

HCID 120623,5-Diaminobenzoic acidHCID 96623Methoxyacetyl chloride

生成物 1

HCID 146992893,5-Bis(methoxyacetylamino)benzoic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 3,5-diaminobenzoic acid (6.1 g) in pyridine (80 ml) is added dropwise methoxyacetyl chloride (8.0 ml) at room temperature, and the mixture is stirred for 2 hours as it stands. From the reaction mixture, pyridine is distilled off under reduced pressure. To the residue is added 1N hydrochloric acid, and the resulting solid substance is separated by filtration and washed with water. The resulting crude crystals are recrystallized from ethanol to give the title compound (8.0 g) having the following physical properties.

後処理

  1. distillationFrom the reaction mixture, pyridine is distilled off under reduced pressure
  2. additionTo the residue is added 1N hydrochloric acid
  3. customthe resulting solid substance is separated by filtration
  4. washwashed with water
  5. customThe resulting crude crystals are recrystallized from ethanol

出典と根拠

ORDレコード
ord-c18d1b63afd146d5bc028e6dfcb1a481
出典データセット
uspto-grants-1990_03
特許番号
US04912135

反応ノート

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