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Hydrochloric Acid → 7-nitro-1H-indole-2-carboxylic acid

HRID 1876309
ノート
印刷プレビュー

反応式

HRID 1876309 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:12]=1[NH:11][C:10]([C:13]([O:15]C)=[O:14])=[CH:9]2)([O-:3])=[O:2].[OH-].[Na+].Cl>O1CCCC1.O>[N+:1]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:12]=1[NH:11][C:10]([C:13]([OH:15])=[O:14])=[CH:9]2)([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18550960Methyl 7-nitro-1h-indole-2-carboxylate

生成物 1

HCID 814097-nitro-1H-indole-2-carboxylic acid収率 99%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 7-nitroindole-2-carboxylate (13 g, 59 mmol) prepared in Preparation 8 was dissolved in a solvent mixture of tetrahydrofuran and water (1:1, 300 ml), and 1N aqueous sodium hydroxide solution (180 ml, 177 mmol) was added thereto. The mixture was stirred for 3 h at room temperature, excess 6N hydrochloric acid solution was added, and the mixture was extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was distilled under reduced pressure to give 7-nitro-1H-indole-2-carboxylic acid (12 g, Yield 99%).

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. distillationThe filtrate was distilled under reduced pressure

出典と根拠

ORDレコード
ord-d86e26509b3d444f9cbc1746388a21f3
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309586B2

反応ノート

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