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Methyl iodide → 7-Methoxy-3-methyl-2-trifluoromethylbenzimidazole

HRID 275792
ノート
印刷プレビュー

反応式

HRID 275792 の反応式
[CH3:1][O:2][C:3]1[C:11]2[NH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[H-].[Na+].[CH3:18]I>O1CCCC1>[CH3:1][O:2][C:3]1[C:11]2[N:10]=[C:9]([C:12]([F:15])([F:13])[F:14])[N:8]([CH3:18])[C:7]=2[CH:6]=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 178488964HCID 178488964、化合物

生成物 1

HCID 183166367-Methoxy-3-methyl-2-trifluoromethylbenzimidazole収率 107.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-methoxy-2-trifluoromethylbenzimidazole (1.4 g) in tetrahydrofuran (40 ml) under nitrogen was added sodium hydride (0.32 g; 60% dispersion in oil). The mixture was stirred for 20 minutes at room temperature before methyl iodide (1.35 g) was added. Stirring was continued overnight. The reaction was quenched by the addition of water (10 ml) and the solvent removed in vacuo. Ethyl acetate (50 ml) was added and the organic layer washed with saturated sodium bicarbonate solution (20 ml), water (20 ml) and brine (20 ml). Drying over anhydrous magnesium sulfate followed by the removal of the solvent in vacuo gave the title compound (1.6 g) as an oil which solidified on standing.

後処理

  1. additionwas added
  2. customThe reaction was quenched by the addition of water (10 ml)
  3. customthe solvent removed in vacuo
  4. additionEthyl acetate (50 ml) was added
  5. washthe organic layer washed with saturated sodium bicarbonate solution (20 ml), water (20 ml) and brine (20 ml)
  6. dry with materialDrying over anhydrous magnesium sulfate
  7. customfollowed by the removal of the solvent in vacuo

出典と根拠

ORDレコード
ord-a444ee7d83814d28be7d6d046cd41d05
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06353010B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート