Methylamine → N-methyl-1H-indole-2-carboxamide

HRID 1710518ノート

反応式

HRID 1710518 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[C:2]1[C:10]([O:12]CC)=O.[CH3:15][NH2:16]>>[CH3:15][NH:16][C:10]([C:2]1[NH:1][C:9]2[C:4]([CH:3]=1)=[CH:5][CH:6]=[CH:7][CH:8]=2)=[O:12]

参加物

3

反応物 2

HCID 6329MethylamineHCID 73125Ethyl indole-2-carboxylate

生成物 1

HCID 12461785N-methyl-1H-indole-2-carboxamide

実験手順

A suspension of ethyl indole-2-carboxylate (25.30 g, 133.7 mmole) in 40% aqueous CH3NH2 (400 mL) was stirred at RT. The flask was tightly stoppered to keep the material inside the flask. As the reaction proceeded the product began to precipitate. The reaction was stirred at RT for 3 days, then was concentrated to remove approximately 200 mL of the solvent. The remaining residue was diluted with H2O (500 mL), and the solid was collected by suction filtration and washed with H2O. Drying under high vacuum left the title compound (21.50 g, 92%) as a light yellow solid: MS (ES) m/e 175 (M+H)+.

後処理

  1. customto precipitate
  2. stirringThe reaction was stirred at RT for 3 days
  3. concentrationwas concentrated
  4. customto remove approximately 200 mL of the solvent
  5. additionThe remaining residue was diluted with H2O (500 mL)
  6. filtrationthe solid was collected by suction filtration
  7. washwashed with H2O
  8. customDrying under high vacuum
  9. waitleft the title compound (21.50 g, 92%) as a light yellow solid

出典と根拠

ORDレコード
ord-b8288ebf735e47b187f5f9864889a71c
出典データセット
uspto-grants-2010_09
特許番号
US07790716B2

反応ノート

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