Hydrazine hydrate (1:1) → 1-Methyl-2-oxo-1,2-dihydropyridine-4-carbohydrazide

HRID 500550ノート

反応式

HRID 500550 の反応式
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][N:8]([CH3:11])[C:7](=[O:12])[CH:6]=1)=O.O.[NH2:14][NH2:15]>C(O)C.C(OCC)C>[CH3:11][N:8]1[CH:9]=[CH:10][C:5]([C:3]([NH:14][NH2:15])=[O:2])=[CH:6][C:7]1=[O:12]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 819408Methyl 1-methyl-2-oxo-1,2-dihydropyridine-4-carboxylate

生成物 1

HCID 431322131-Methyl-2-oxo-1,2-dihydropyridine-4-carbohydrazide収率 78%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
78 °C

実験手順

The title compound from example 30.1 (4 g, 24 mmol) was dissolved in ethanol and stirred at 78° C. Hydrazine hydrate (5.8 mL, 120 mmol) was added via a syringe and the reaction was stirred for 3 h at 78° C., at which time the starting material was no longer visible by TLC. The reaction mixture (clear solution) was then cooled to room temperature, and diluted with diethyl ether to precipitate the product which was collected by vacuum filtration to yield the title compound as a pale yellow solid (3.13 g, 78%).

後処理

  1. stirringthe reaction was stirred for 3 h at 78° C., at which time the starting material
  2. temperatureThe reaction mixture (clear solution) was then cooled to room temperature
  3. customto precipitate the product which
  4. filtrationwas collected by vacuum filtration

出典と根拠

ORDレコード
ord-e1a49d0a4fd34ae4a7b28283f5fd8679
出典データセット
uspto-grants-2010_08
特許番号
US07772235B2

反応ノート

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