HCID 178526787, 화합물 → HCID 178508009, 화합물

HRID 1435578노트

반응식

HRID 1435578 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[N:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[NH:10][C:7]2=[N:8][CH:9]=1)([O-])=O>C(O)(=O)C.[Fe]>[C:13]1([C:11]2[NH:10][C:7]3=[N:8][CH:9]=[C:4]([NH2:1])[CH:5]=[C:6]3[N:12]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

4

반응물 1

HCID 178526787HCID 178526787, 화합물

생성물 1

HCID 178508009HCID 178508009, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

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온도
80 °C

실험 절차

12.0 g 6-nitro-2-phenyl-3H-imidazo[4,5-b]pyridine were dissolved in 1 l acetic acid. 18 g iron powder were added and the mixture heated to 80° C. with stirring. After 2 hrs the mixture was cooled to room temperature and filtered over Celite. The celite pad was washed with methanol and the combined filtrates were evaporated. The residue was dissolved methanol/dichloromethane 1:1 and filtered over silica. The filtrate was concentrated to a volume of 100 ml, the resulting precipitate collected by filtration and washed with methanol. Yield 7.68 g

후처리

  1. temperatureAfter 2 hrs the mixture was cooled to room temperature
  2. filtrationfiltered over Celite
  3. washThe celite pad was washed with methanol
  4. customthe combined filtrates were evaporated
  5. dissolutionThe residue was dissolved methanol/dichloromethane 1:1
  6. filtrationfiltered over silica
  7. concentrationThe filtrate was concentrated to a volume of 100 ml
  8. filtrationthe resulting precipitate collected by filtration
  9. washwashed with methanol

출처 및 근거

ORD 기록
ord-e706b720c0a443c0bb5ab8df43b8ff5b
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618964B2

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