Water → HCID 178509651、化合物

HRID 976576ノート

反応式

HRID 976576 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-0b206c4cb23241d09f7958fdf1d6e38a
出典データセット
uspto-grants-1997_03
特許番号
US05612360

反応ノート

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