HCID 178526787, 화합물 → HCID 178508009, 화합물

HRID 502792노트

반응식

HRID 502792 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

반응 조건

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.

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-00b742234d8d4c81b39a6c19ee4abf03
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776878B2

반응 노트

불러오는 중…