Boron trifluoride etherate → HCID 15158051, Verbindung

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Reaktionsgleichung

[CH:1]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])OCC.B(F)(F)F.CCOCC.[N:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[C:26](=[O:34])[CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][N:29]=1.C(N(C(C)C)CC)(C)C.C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[CH2:9]([O:8][CH:1]([O:5][CH2:6][CH3:7])[CH:27]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][N:29]=1)[C:26]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][N:20]=1)=[O:34])[CH3:10]

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

A solution of 15 mL (0.089 mol) of triethyl orthoformate in 100 mL of methylene chloride was stirred under nitrogen at -78° C. and 13.2 mL (0.108 mol) of boron trifluoride etherate was added. The solution was allowed to warm to 0° C., recooled to -78° C., and a solution of 8.0 g (0.04 mol) of 1.2-bis(2-pyridinyl)ethanone in 75 mL of methylene chloride was added, followed after 30 min by 22 mL (0.132 mol) of diisopropylethylamine in 30 mL of methylene chloride. The reaction was stirred 45 min at -78° C., poured into 400 mL of water containing 10 g of NaHCO3 and stirred 20 min. The phases were separated, the methylene chloride layer was dried over MgSO4 and stripped to yield about 17 g of crude 3,3-diethoxy-1,2-bis(2-pyridinyl)-1-propanone.

Aufarbeitung

customrecooled to -78° C.
stirringstirred 20 min
customThe phases were separated
dry with materialthe methylene chloride layer was dried over MgSO4

Quellen und Nachweise

ORD-Eintrag: ord-1aae487049d244c182c83ceb84504e62
Quelldatensatz: uspto-grants-1990_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04925857

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