Methyl iodide → 2-Methoxy-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-pyridine

HRID 500545노트

반응식

HRID 500545 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[N:10]([CH3:15])[C:11]([SH:14])=[N:12][N:13]=2)[CH:6]=[CH:5][N:4]=1.I[CH3:17]>[OH-].[Na+].C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[N:10]([CH3:15])[C:11]([S:14][CH3:17])=[N:12][N:13]=2)[CH:6]=[CH:5][N:4]=1

참가 물질

5

반응물 2

HCID 6328Methyl iodideHCID 178488243HCID 178488243, 화합물

생성물 1

HCID 248517082-Methoxy-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-pyridine수율 97.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

The title compound of example 24.1 (21.30 g, 95.83 mmol) was set stirring in 1 M sodium hydroxide in a cold water bath. Iodomethane (21.76 g, 153.3 mmol) in ethanol (63 mL) was added to the reaction. As the reaction progressed, solid began to precipitate out. The reaction was allowed to stir at RT for 12 hours. The reaction mixture was extracted with dichloromethane and the organic extracts were washed with brine, dried and concentrated to afford the title compound as a white solid (22 g, 97%).

후처리

  1. customto precipitate out
  2. extractionThe reaction mixture was extracted with dichloromethane
  3. washthe organic extracts were washed with brine
  4. customdried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-61e32176a0d44470aed2709f2325e35b
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772235B2

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