Ammonia → HCID 67027581、化合物

HRID 2400360ノート

反応式

HRID 2400360 の反応式
[N:1]1[CH:2]=[CH:3][N:4]2[CH:9]=[CH:8][C:7]([C:10]([NH:12][NH2:13])=O)=[CH:6][C:5]=12.[CH3:14][C:15]([CH:17]=O)=O.[NH3:19]>C(O)C>[CH3:14][C:15]1[N:19]=[C:10]([C:7]2[CH:8]=[CH:9][N:4]3[CH:3]=[CH:2][N:1]=[C:5]3[CH:6]=2)[N:12]=[N:13][CH:17]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 880MethylglyoxalHCID 55281632Imidazo(1,2-a)pyridine-7-carbohydrazide

生成物 1

HCID 67027581HCID 67027581、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of imidazo[1,2-a]pyridine-7-carboxylic acid hydrazide (705 mg, 4.0 mmol, 1.0 equiv) and pyruvic aldehyde (40 wt % in water, 0.8 ml) in ethanol (10 ml) was stirred at room temperature for 2.5 hours. Ammonia (2M in methanol, 10 ml) was added and stirred at room temperature for 15 minutes before heating to 100 deg C. in a microwave for 60 minutes. The reaction mixture was concentrated in vacuo and dichloromethane was added. After stirring at room temperature for 15 minutes the solid (recovered starting material) was filtered off and the liquors were purified by column chromatography (0-10% methanol/dichloromethane) furnishing 200 mg of a yellow solid. MS: [M+H]+212

後処理

  1. stirringstirred at room temperature for 15 minutes
  2. temperaturebefore heating to 100 deg C
  3. waitin a microwave for 60 minutes
  4. concentrationThe reaction mixture was concentrated in vacuo and dichloromethane
  5. additionwas added
  6. stirringAfter stirring at room temperature for 15 minutes
  7. customthe solid (recovered starting material)
  8. filtrationwas filtered off
  9. customthe liquors were purified by column chromatography (0-10% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-55f02ad8d5b8411f8dfede7065b1320b
出典データセット
uspto-grants-2014_08
特許番号
US08796244B2

反応ノート

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