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Cesium carbonate → Methyl 3-{6-[(diphenylmethylene)amino]pyridazin-4-yl}benzoate

HRID 407074
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HRID 407074 반응식
Cl[C:2]1[N:7]=[N:6][CH:5]=[C:4]([C:8]2[CH:9]=[C:10]([CH:15]=[CH:16][CH:17]=2)[C:11]([O:13][CH3:14])=[O:12])[CH:3]=1.[C:18](=[NH:31])([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.C(OCC)(=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1C=CC(P(C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:19]1([C:18](=[N:31][C:2]2[N:7]=[N:6][CH:5]=[C:4]([C:8]3[CH:9]=[C:10]([CH:15]=[CH:16][CH:17]=3)[C:11]([O:13][CH3:14])=[O:12])[CH:3]=2)[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 10796Cesium carbonateHCID 136809Benzophenone imineHCID 86667186Methyl 3-(6-chloropyridazin-4-yl)benzoate

생성물 1

HCID 86667185Methyl 3-{6-[(diphenylmethylene)amino]pyridazin-4-yl}benzoate수율 69.6%

시약·촉매·용매 4

HCID 167845palladium(II) acetate촉매
HCID 634876
Binap, (A+-)-
촉매
HCID 8857Ethyl Acetate용매
HCID 312751,4-Dioxane용매

반응 조건

온도
110 °C

실험 절차

A mixture of methyl 3-(6-chloropyridazin-4-yl)benzoate (0.21 g, 0.84 mmol), benzophenone imine (260 μL, 1.5 mmol), (R)-(+)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (26 mg, 0.042 mmol), cesium carbonate (0.55 g, 1.7 mmol) and palladium acetate (9.5 mg, 0.042 mmol) in 1,4-dioxane (3 mL) was vacuum and refilled with nitrogen for 3 times. The reaction was stirred at 110° C. overnight. After cooling it was diluted with ethyl acetate. The organic solution was washed with water and brine, dried over Na2SO4. After filtration the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with ethyl acetate in methylene chloride (0-20%) to afford the desired product (0.23 g). LCMS (M+H)+: m/z=394.2

후처리

  1. additionrefilled with nitrogen for 3 times
  2. temperatureAfter cooling it
  3. washThe organic solution was washed with water and brine
  4. dry with materialdried over Na2SO4
  5. filtrationAfter filtration the filtrate
  6. concentrationwas concentrated under reduced pressure
  7. customThe residue was purified by flash chromatography on a silica gel column with ethyl acetate in methylene chloride (0-20%)

출처 및 근거

ORD 기록
ord-bc17eb2769874d5aaed9652464303362
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08754114B2

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