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

HRID 500552노트

반응식

HRID 500552 반응식
[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]

참가 물질

6

반응물 4

HCID 702EthanolHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 178481695HCID 178481695, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-21cd996aec87452e82cc17978abd2a69
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772235B2

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