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Hydrochloric Acid → HCID 178524942, 화합물

HRID 82064
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HRID 82064 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]([O:13]C)=[O:12])=[N:9][NH:8][C:5]2=[N:6][CH:7]=1.Cl>[OH-].[Na+]>[Br:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]([OH:13])=[O:12])=[N:9][NH:8][C:5]2=[N:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178499173HCID 178499173, 화합물

생성물 1

HCID 178524942HCID 178524942, 화합물수율 92.6%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
90 °C

실험 절차

A suspension of methyl 5-bromo-1H-pyrazolo[3,4-b]pyridine-3-carboxylate (VII) (70 mg, 0.27 mmol) in aqueous 1N NaOH solution (20 mL) was heated at 90° C. for 3 h until the solution became clear. The solution was then cooled to 0° C. and acidified with a 10% HCl solution. The solids formed were filtered, washed with cold water and dried at room temperature under vacuum to give 5-bromo-1H-pyrazolo[3,4-b]pyridine-3-carboxylic acid (VIII) as a white solid (60 mg, 0.25 mmol, 92% yield). 1H NMR (CDCl3) δ ppm 8.58 (d, J=3.01 Hz, 1 H), 8.66 (d, J=3.01 Hz, 1 H); ESIMS Found for C7H4BrN3O2 m/z 242.1 (M+H).

후처리

  1. temperatureThe solution was then cooled to 0° C.
  2. customThe solids formed
  3. filtrationwere filtered
  4. washwashed with cold water
  5. customdried at room temperature under vacuum

출처 및 근거

ORD 기록
ord-c681cb20a78e4475889789f2d8db6dd9
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846714B2

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