Hydrazine hydrate (1:1) → HCID 178489372, 화합물

HRID 886614노트

반응식

HRID 886614 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])=O)[C:5](F)=[N:6][CH:7]=1.O.[NH2:20][NH2:21]>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[O:17][CH3:18])=[N:21][NH:20][C:5]2=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 59825042(5-Bromo-2-fluoro-pyridin-3-yl)-(2-methoxy-phenyl)-methanone

생성물 1

HCID 178489372HCID 178489372, 화합물수율 59.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of (5-bromo-2-fluoro-pyridin-3-yl)-(2-methoxy-phenyl)-methanone (1.9 g, 6.1 mmol) in ethanol (125 ml), hydrazine monohydrate (691 μl, 12.2 mmol) was added and the resulting solution was allowed to stir at room temperature overnight. Solvent was removed under reduced pressure and the product was precipitated out by addition of water to afford 5-bromo-3-(2-methoxy-phenyl)-1H-pyrazolo[3,4-b]pyridine (1.1 g, 58% yield). 1H NMR (500 MHz, DMSO-d6) δ 3.84 (s, 3H), 7.07 (m, 1H), 7.20 (d, 1H), 7.45 (m, 1H), 7.62 9d, 1H), 8.34 (s, 1H), 8.60 (s, 1H). MS: m/z 304+306 (M+H+).

후처리

  1. customSolvent was removed under reduced pressure
  2. customthe product was precipitated out by addition of water

출처 및 근거

ORD 기록
ord-40d66947a7b4475995b3bf1fb3ee00a0
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242280B2

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