Formic Acid → HCID 21468861、化合物

HRID 743865ノート

反応式

HRID 743865 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].[CH:17](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[N:8]=[CH:17][NH:1][C:2]=2[CH:3]=1)#[N:12]

参加物

3

反応物 2

HCID 284Formic AcidHCID 21468845HCID 21468845、化合物

生成物 1

HCID 21468861HCID 21468861、化合物

実験手順

2-(3,4-Diaminophenyl)benzonitrile (0.04 moles, 8.3 g) was refluxed in 100 ml formic acid for 3 hours. The solution was concentrated in vacuo, triturated with toluene, and dissolved in water. The pH of the solution was adjusted to 7.5 with 2N sodium hydroxide. The intermediate was extracted with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated in vacuo. The solid was triturated with 25% ethyl acetate/75% hexane, filtered and purified by HPLC on silica gel eluted with a gradient of 50-75% ethyl acetate in hexane. The reaction yielded 7.3 g of 5-(2-Cyanophenyl)benzimidazole. (MS)

後処理

  1. concentrationThe solution was concentrated in vacuo
  2. customtriturated with toluene
  3. dissolutiondissolved in water
  4. extractionThe intermediate was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe solid was triturated with 25% ethyl acetate/75% hexane
  8. filtrationfiltered
  9. custompurified by HPLC on silica gel
  10. washeluted with a gradient of 50-75% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-45a51d30f21941f197883106d6b8f229
出典データセット
uspto-grants-1996_09
特許番号
US05556981

反応ノート

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