Formic Acid → HCID 21468861, 화합물

HRID 743865노트

반응식

HRID 743865 반응식
[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]

참가 물질

3

반응물 2

HCID 284Formic AcidHCID 21468845HCID 21468845, 화합물

생성물 1

HCID 21468861HCID 21468861, 화합물

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-45a51d30f21941f197883106d6b8f229
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556981

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