Hydrazine → 4-(5-amino-6-(hydrazinecarbonyl)pyrazin-2-yl)-N,N-dimethylbenzamide

HRID 2204814

反応式

HRID 2204814 の反応式
[NH2:1][C:2]1[C:3]([C:19]([O:21]C)=O)=[N:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14](=[O:18])[N:15]([CH3:17])[CH3:16])=[CH:10][CH:9]=2)=[CH:6][N:7]=1.[NH2:23][NH2:24]>CCO>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]([C:14]([N:15]([CH3:16])[CH3:17])=[O:18])=[CH:12][CH:13]=2)=[N:4][C:3]=1[C:19]([NH:23][NH2:24])=[O:21]

参加物

4

反応物 2

HCID 9321HydrazineHCID 59471801Methyl 3-amino-6-(4-(dimethylcarbamoyl)phenyl)pyrazine-2-carboxylate

生成物 1

HCID 594716414-(5-amino-6-(hydrazinecarbonyl)pyrazin-2-yl)-N,N-dimethylbenzamide収率 87%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of methyl 3-amino-6-[4-(dimethylcarbamoyl)phenyl]pyrazine-2-carboxylate (1.7011 g, 5.664 mmol) in EtOH (10.21 mL) was added hydrazine (726.1 mg, 711.2 μL, 22.66 mmol). The resultant solution was heated to reflux for 30 minutes and then allowed to cool to RT. The precipitate was filtered off and dried (1.47 g, 87% Yield). 1H NMR (400.0 MHz, DMSO) d 2.96 (s, 3H), 3.00 (s, 3H), 4.58 (d, J=4.4 Hz, 2H), 7.46 (d, J=8.4 Hz, 2H), 8.27-8.29 (m, 2H), 8.88 (s, 1H) and 10.09 (s, 1H) ppm; MS (ES+) 301.13

後処理

  1. temperatureto reflux for 30 minutes
  2. filtrationThe precipitate was filtered off
  3. customdried (1.47 g, 87% Yield)

出典と根拠

ORDレコード
ord-e076cb99ece64ecaac1675eddb49a9b1
出典データセット
uspto-grants-2016_06
特許番号
US09365557B2

関連ノート

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