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Potassium Carbonate → 3-(difluoromethyl)-6-(3,4-dimethoxyphenyl)-3H-imidazo[4,5-c]pyridin-4(5H)-one

HRID 2209002
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HRID 2209002 반응식
C([O:8][C:9]1[C:14]2[N:15]([CH:18]([F:20])[F:19])[CH:16]=[N:17][C:13]=2[CH:12]=[C:11](Cl)[N:10]=1)C1C=CC=CC=1.[CH3:22][O:23][C:24]1[CH:25]=[C:26](B(O)O)[CH:27]=[CH:28][C:29]=1[O:30][CH3:31].C([O-])([O-])=O.[K+].[K+].B(O)O.C([O-])=O.[NH4+]>C1(C)C=CC=CC=1.O.CCOC(C)=O.CCO.CN(C=O)C.CC(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)C.CC(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)C.Cl[Pd]Cl.[OH-].[OH-].[Pd+2]>[F:20][CH:18]([F:19])[N:15]1[C:14]2[C:9](=[O:8])[NH:10][C:11]([C:27]3[CH:26]=[CH:25][C:24]([O:23][CH3:22])=[C:29]([O:30][CH3:31])[CH:28]=3)=[CH:12][C:13]=2[N:17]=[CH:16]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

13

반응물 5

HCID 11430Potassium Carbonate2회HCID 61668Boronic AcidHCID 2723923Ammonium formateHCID 27347023,4-Dimethoxyphenylboronic acidHCID 1178440534-(benzyloxy)-6-chloro-3-(difluoromethyl)-3H-imidazo[4,5-c]pyridine

생성물 1

HCID 1178438163-(difluoromethyl)-6-(3,4-dimethoxyphenyl)-3H-imidazo[4,5-c]pyridin-4(5H)-one

시약·촉매·용매 7

HCID 9942167Palladium hydroxide촉매HCID 11714597Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II)촉매HCID 702Ethanol용매HCID 962Water용매3회HCID 1140Toluene용매2회HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매

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온도
90 °C

실험 절차

4-(benzyloxy)-6-chloro-3-(difluoromethyl)-3H-imidazo[4,5-c]pyridine 2.28 (113 mg, 0.365 mmol), 3,4-dimethoxyphenylboronic acid (107 mg, 0.588 mmol), bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (14.5 mg, 0.0205 mmol) and K2CO3 (164 mg, 1.19 mmol) were taken up in toluene (3 mL) and water (0.6 mL) under Ar. The stirred mixture was heated to 90° C. After 3.5 h, additional boronic acid (35 mg, 0.19 mmol), catalyst (4.5 mg, 0.0064 mmol), and K2CO3 (53 mg, 0.38 mmol) were added as a suspension in toluene (1 mL) and water (0.3 mL). After an additional 1 h, the reaction mixture was cooled to r.t. and was diluted with EtOAc (20 mL) and water (20 mL). The phases were separated, and the aqueous phase was extracted with EtOAc (20 mL). The organic phase was dried over Na2SO4, filtered, and concentrated onto silica gel. Purification by silica gel chromatography (20% to 50% acetone in hexanes) provided a residue that was dissolved in EtOH (3 mL) and DMF (2 mL). Ammonium formate (260 mg, 4.1 mmol) and Pd(OH)2 on carbon (20 wt. % Pd, 40 mg) were added and the mixture was heated to 70° C. and stirred for 20 min. The mixture was diluted with DMF (5 mL) and filtered through Celite. The filtrate was concentrated in vacuo and the resulting crude solid was purified by silica gel chromatography (0% to 10% MeOH in DCM) to provide 3-(difluoromethyl)-6-(3,4-dimethoxyphenyl)-3H-imidazo[4,5-c]pyridin-4(5H)-one 2.29.

후처리

  1. waitAfter an additional 1 h
  2. temperaturethe reaction mixture was cooled to r.t.
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with EtOAc (20 mL)
  5. dry with materialThe organic phase was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated onto silica gel
  8. customPurification by silica gel chromatography (20% to 50% acetone in hexanes)
  9. customprovided a residue that
  10. temperaturethe mixture was heated to 70° C.
  11. filtrationfiltered through Celite
  12. concentrationThe filtrate was concentrated in vacuo
  13. customthe resulting crude solid was purified by silica gel chromatography (0% to 10% MeOH in DCM)

출처 및 근거

ORD 기록
ord-448a3a01bc994e6eaf3b25defebcc074
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376441B2

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