Hydroxylamine → 4-(6-Bromo-1-phenyl-1H-imidazo[4,5-c]pyridin-2-yl)-furazan-3-amine

HRID 1986369노트

반응식

HRID 1986369 반응식
[Br:1][C:2]1[N:7]=[CH:6][C:5]2[N:8]=[C:9]([C:17](=[N:20][OH:21])[C:18]#[N:19])[N:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1.C([N:24](CC)CC)C.NO.O>C1COCC1>[Br:1][C:2]1[N:7]=[CH:6][C:5]2[N:8]=[C:9]([C:17]3[C:18]([NH2:24])=[N:19][O:21][N:20]=3)[N:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1

참가 물질

6

반응물 4

HCID 787HydroxylamineHCID 962WaterHCID 8471TriethylamineHCID 136384883(6-Bromo-1-phenyl-1H-imidazo[4,5-c]pyridin-2-yl)(hydroxyimino)acetonitrile

생성물 1

HCID 866233484-(6-Bromo-1-phenyl-1H-imidazo[4,5-c]pyridin-2-yl)-furazan-3-amine수율 60%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
120 °C

실험 절차

The product from Step 6 (2.7 g, 7.93 mmol) in THF (5 mL) and triethylamine (1.1 mL, 7.93 mmol) was treated with a 50% solution of hydroxylamine in water (0.24 mL, 7.93 mmol). The mixture was heated at 120° C. in a sealed tube for 10 h and the reaction allowed to cool to room temperature. The resulting precipitate was filtered and dried in vacuo to afford the title compound (1.7 g, 60%). MS (ES+) m/e 357/359 [M+H]+.

후처리

  1. temperatureto cool to room temperature
  2. filtrationThe resulting precipitate was filtered
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-fb2d6472c7dd4149b089675262f2d8b4
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07547779B2

반응 노트

불러오는 중…