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

HRID 500545ノート

反応式

HRID 500545 の反応式
[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

参加物

5

反応物 2

HCID 6328Methyl iodideHCID 178488243HCID 178488243、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-61e32176a0d44470aed2709f2325e35b
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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