Water → HCID 178509651、化合物

HRID 866248ノート

反応式

HRID 866248 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=2[C:11]#[N:12])[CH:5]=[CH:6][C:7]=1[NH2:8].O.[F:18][C:19]([F:24])([F:23])[C:20](O)=O>>[C:11]([C:10]1[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=1[C:4]1[CH:5]=[CH:6][C:7]2[NH:8][C:20]([C:19]([F:24])([F:23])[F:18])=[N:1][C:2]=2[CH:3]=1)#[N:12]

参加物

4

反応物 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 21468845HCID 21468845、化合物

生成物 1

HCID 178509651HCID 178509651、化合物

反応条件

温度
85 °C

実験手順

2-(3,4-Diaminophenyl)benzonitrile (0.01 moles, 2.09 g) was dissolved in 10 ml trifluoroacetic acid and heated at 85° C. for 16 hours. The solution was poured into water and extracted with ethyl acetate. The pH was adjusted to 3.0 using 5N NaOH. The ethyl acetate was washed with brine, dried over sodium sulfate, and concentrated. The residue was chromatographed on silica gel eluted with 25 % ethyl acetate in hexane. The reaction yielded 2.05 g of 5-(2-cyanophenyl)-2-trifluoromethyl-1H-benzimidazole. (MS)

後処理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate was washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel
  6. washeluted with 25 % ethyl acetate in hexane

出典と根拠

ORDレコード
ord-5c7d96cc7ffd402cb77dc5ad30d5f663
出典データセット
uspto-grants-1996_10
特許番号
US05569768

反応ノート

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