Methyl iodide → HCID 19866681、化合物

HRID 1199464ノート

反応式

HRID 1199464 の反応式
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[NH:13][C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[N:10]=1.CI.[C:20](=O)([O-])[O-].[K+].[K+]>CN(C)C=O.[Cl-].[Na+].O>[CH3:20][N:13]1[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[N:10]=[C:9]1[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[S:2][CH3:1]

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 123160831H-Benzimidazole, 2-[2-(methylthio)phenyl]-

生成物 1

HCID 19866681HCID 19866681、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

The product of step (a) above (3.25 g), methyl iodide (1.92 g) and potassium carbonate (5.2 g) were stirred together in dry dimethylformamide (50 ml) at room temperature for 24 hours. The reaction mixture was poured into brine and extracted into ethyl acetate, the extract was washed with excess brine, dried over magnesium sulphate and evaporated to dryness in vacuo and the residue was purified by flash chromatography (SiO2 /CH2Cl2 9:1 ethyl acetate) to afford the sub-title compound as yellow solid, MS MW 254 bp 239.

後処理

  1. extractionextracted into ethyl acetate
  2. washthe extract was washed with excess brine
  3. dry with materialdried over magnesium sulphate
  4. customevaporated to dryness in vacuo
  5. customthe residue was purified by flash chromatography (SiO2 /CH2Cl2 9:1 ethyl acetate)

出典と根拠

ORDレコード
ord-42976fe0c28b40e28a0f396355ff0402
出典データセット
uspto-grants-1990_02
特許番号
US04900751

反応ノート

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