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Tetrahydrofuran → Ethyl 4-amino-1-methyl-1H-indole-2-carboxylate

HRID 565018
ノート
印刷プレビュー

反応式

HRID 565018 の反応式
O1CCCC1.[CH3:6][N:7]1[C:15]2[C:10](=[C:11]([N+:16]([O-])=O)[CH:12]=[CH:13][CH:14]=2)[CH:9]=[C:8]1[C:19]([O:21][CH2:22][CH3:23])=[O:20]>[Pd].CO>[NH2:16][C:11]1[CH:12]=[CH:13][CH:14]=[C:15]2[C:10]=1[CH:9]=[C:8]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[N:7]2[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8028TetrahydrofuranHCID 13401551HCID 13401551、化合物

生成物 1

HCID 13401554Ethyl 4-amino-1-methyl-1H-indole-2-carboxylate収率 99.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

In a solvent mixture of 50 ml of tetrahydrofuran and 50 ml of methanol was dissolved 1.37 g (5.52 mmol) of ethyl 1-methyl-4-nitro-2-indolecarboxylate. Thereafter 0.30 g of 10% palladium/carbon was added to the solution and catalytic hydrogenation was then conducted at ambient temperature under normal pressure. After completion of the reaction, the catalyst was filtered off and the filtrate was then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to give 1.2 g (>99%) of ethyl 4-amino-1-methyl-2-indolecarboxylate.

後処理

  1. customwas then conducted at ambient temperature under normal pressure
  2. customAfter completion of the reaction
  3. filtrationthe catalyst was filtered off
  4. concentrationthe filtrate was then concentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-4beba09550b1469db626b8c0dea60c28
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06169107A

反応ノート

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