Ethanol → 1-Methyl-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-1h-pyridin-2-one

HRID 500552ノート

反応式

HRID 500552 の反応式
[SH:1][C:2]1[N:3]([CH3:15])[C:4]([C:7]2[CH:12]=[CH:11][N:10]([CH3:13])[C:9](=[O:14])[CH:8]=2)=[N:5][N:6]=1.[OH-].[Na+].[CH2:18](O)C.IC>O>[CH3:13][N:10]1[CH:11]=[CH:12][C:7]([C:4]2[N:3]([CH3:15])[C:2]([S:1][CH3:18])=[N:6][N:5]=2)=[CH:8][C:9]1=[O:14]

参加物

6

反応物 4

HCID 702EthanolHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 178481695HCID 178481695、化合物

生成物 1

HCID 248520611-Methyl-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-1h-pyridin-2-one収率 78%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

The title compound from example 32.1 (600 mg, 2.7 mmol) was dissolved in a solution of sodium hydroxide (216 mg, 5.4 mmol) and water (5 mL). When a clear, uniform solution was observed ethanol (6 mL) was added, followed by iodomethane (268 μL, 4.3 mmol). The reaction was stirred at room temperature for 6 h. The reaction mixture was then diluted with water and extracted four times with chloroform. The organic phase was dried over magnesium sulfate, filtered and concentrated to yield the title compound (yellowish solid, 500 mg, 78%).

後処理

  1. additionwas added
  2. extractionextracted four times with chloroform
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-21cd996aec87452e82cc17978abd2a69
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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