Hydrochloric Acid → HCID 86606798, 화합물

HRID 42595노트

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HRID 42595 반응식
C([O:3][CH:4](OCC)[CH2:5][N:6]1[CH:14]=[C:13]2[C:8]([N:9]=[C:10]([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[C:11]([C:22]3[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=3)=[C:12]2[C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)=[N:7]1)C.Cl>>[F:21][C:18]1[CH:19]=[CH:20][C:15]([C:12]2[C:13]3[C:8](=[N:7][N:6]([CH2:5][CH:4]=[O:3])[CH:14]=3)[N:9]=[C:10]([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[C:11]=2[C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)=[CH:16][CH:17]=1

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 684434952-(2,2-Diethoxyethyl)-4,6-bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridine

생성물 1

HCID 86606798HCID 86606798, 화합물수율 65%

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온도
100 °C

실험 절차

In a volumetric flask, 2-(2,2-diethoxyethyl)-4,6-bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridine (0.31 g, 0.6 mmol, obtained in example 73) and 1 N HCl (2.6 mL) were introduced. The mixture was heated to 100° C. for 1 hour. It was allowed to cool, adjusted to pH=7 and extracted with EtOAc. The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity eluent, to afford 166 mg of the title compound (yield: 65%).

후처리

  1. temperatureto cool
  2. extractionextracted with EtOAc
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated to dryness
  5. customThe crude product obtained
  6. customwas purified by chromatography on silica gel
  7. temperatureof increasing polarity eluent

출처 및 근거

ORD 기록
ord-a816b7e7d0d5449ab9764d09d3403a06
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536194B2

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