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Methyl 4-bromobenzoate → HCID 22730763, 화합물

HRID 1427000
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HRID 1427000 반응식
[C:1]([N:8]1[CH2:13][CH:12]=[C:11](B2OC(C)(C)C(C)(C)O2)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].Br[C:24]1[CH:33]=[CH:32][C:27]([C:28]([O:30][CH3:31])=[O:29])=[CH:26][CH:25]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C(=O)(O)[O-].[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(OCC)(=O)C.O.C(O)C.C1(C)C=CC=CC=1>[CH3:31][O:30][C:28]([C:27]1[CH:32]=[CH:33][C:24]([C:11]2[CH2:10][CH2:9][N:8]([C:1]([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2])[CH2:13][CH:12]=2)=[CH:25][CH:26]=1)=[O:29]
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참가 물질

11

반응물 5

HCID 12081Methyl 4-bromobenzoateHCID 62657Potassium Phosphate, TribasicHCID 516892Sodium BicarbonateHCID 4642098Tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,6-tetrahydropyridine-1-carboxylateHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl

생성물 1

HCID 22730763
HCID 22730763, 화합물
수율 96.6%

시약·촉매·용매 5

HCID 167845palladium(II) acetate촉매HCID 702Ethanol용매HCID 962Water용매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

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온도
90 °C

실험 절차

Toluene (20 mL), ethanol (6 mL), and water (2 mL) were added to commercially available 1-N—BOC-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-3,6-dihydro-2H-pyridine (1.00 g, 3.23 mmol), methyl 4-bromobenzoate (695 mg, 3.23 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxy biphenyl (266 mg, 0.65 mmol), palladium(II) acetate (73 mg, 0.32 mmol), and tripotassium phosphate (2.06 g, 9.70 mmol) under nitrogen atmosphere, and the mixture was stirred at 90° C. for 5 hours. The reaction mixture was cooled to room temperature and a saturated aqueous sodium bicarbonate solution and ethyl acetate were added for partition. The aqueous layer was extracted with ethyl acetate three times and then the organic layer was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated and the resultant residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=19:1-13:7) to obtain the title compound (0.99 g, 96%).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customfor partition
  3. extractionThe aqueous layer was extracted with ethyl acetate three times
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customThe solvent was evaporated
  7. customthe resultant residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=19:1-13:7)

출처 및 근거

ORD 기록
ord-2ec424bbd8e84c82b376f7a6194b340a
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933099B2

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