Diiodomethane → 4-[1-(4-Fluorophenoxymethyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

HRID 132004ノート

反応式

HRID 132004 の反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[C:11]([NH2:15])=[N:12][O:13][N:14]=1.[C:16](=[O:19])([O-])[O-].[K+].[K+].[F:22][C:23]1[CH:28]=[CH:27][C:26](O)=[CH:25][CH:24]=1.ICI>>[F:22][C:23]1[CH:28]=[CH:27][C:26]([O:19][CH2:16][N:3]2[C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:1]=[C:2]2[C:10]2[C:11]([NH2:15])=[N:12][O:13][N:14]=2)=[CH:25][CH:24]=1

参加物

5

反応物 4

HCID 6346DiiodomethaneHCID 97324-FluorophenolHCID 11430Potassium CarbonateHCID 7385314-(1H-benzimidazol-2-yl)-1,2,5-oxadiazol-3-amine

生成物 1

HCID 674581694-[1-(4-Fluorophenoxymethyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

実験手順

To a solution of 4-(1H-benzimidazol-2-yl)-furazan-3-ylamine (0.10 g, 0.497 mmol) is added potassium carbonate (0.172 g, 1.24 mmol) followed by 4-fluorophenol (0.0557 g, 0.497 mmol) and diiodomethane (0.133 g, 0.497 mmol). The mixture is stirred over night. Evaporation of the solvent under reduced pressure and partitioning of the resulting residue between water and ethyl acetate followed by drying of the organic solution over sodium sulphate and chromatography of the residue gives the title compound as a colorless solid, m.p. 155-158° C.

後処理

  1. customEvaporation of the solvent under reduced pressure
  2. custompartitioning of the resulting residue between water and ethyl acetate
  3. dry with materialby drying of the organic solution over sodium sulphate and chromatography of the residue

出典と根拠

ORDレコード
ord-4ee40691d57146eea138828ba17bbfdf
出典データセット
uspto-grants-2008_06
特許番号
US07385061B2

反応ノート

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