Hydrochloric Acid → 2-(((Benzyloxy)carbonyl)amino)-5-hydroxybenzoic acid

HRID 275832

反応式

HRID 275832 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[C:12](Cl)([O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:13].Cl>[OH-].[Na+]>[CH2:15]([O:14][C:12]([NH:1][C:2]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5])=[O:13])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10387Benzyl chloroformateHCID 1645925-Hydroxyanthranilic acid

生成物 1

HCID 183153542-(((Benzyloxy)carbonyl)amino)-5-hydroxybenzoic acid収率 51.5%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

2-Amino-5-hydroxy-benzoic acid (3.0 g) was dissolved in a 1N aqueous solution of sodium hydroxide (50 ml), to which was added dropwise carbobenzyloxy chloride (3.5 g). The mixture was stirred for one hour at room temperature, which was neutralized with 1N hydrochloric acid, followed by extraction with ethyl acetate (100 ml). The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled under reduced pressure to leave 2-benzyloxycarbonylamino-5-hydroxybenzoic acid as blackish brown crystals (2.9 g).

後処理

  1. extractionfollowed by extraction with ethyl acetate (100 ml)
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled under reduced pressure

出典と根拠

ORDレコード
ord-376d0988882649fe9f625f30c1039e18
出典データセット
uspto-grants-2002_03
特許番号
US06352982B1

関連ノート

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