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

HRID 500550노트

반응식

HRID 500550 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

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온도
78 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-e1a49d0a4fd34ae4a7b28283f5fd8679
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772235B2

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