Methanol → 4-(Dimethylamino)-1,1-dimethoxybut-3-en-2-one
Reaktionsgleichung
[CH3:1][O:2][C:3]([O:7][CH3:8])(C)[CH:4]=[O:5].CO[CH:11](OC)[N:12]([CH3:14])[CH3:13].[CH3:17]O>>[CH3:13][N:12]([CH3:14])[CH:11]=[CH:17][C:4](=[O:5])[CH:3]([O:7][CH3:8])[O:2][CH3:1]Komponenten
4
Versuchsvorschrift
300 g (3.07 ml, 2.54 mol) of methylglyoxal dimethyl acetal (21) were stirred at 110° C. for 4 ours (h), together with 303 g (337 ml, 2.54 mol) of N,N-dimethylformamide dimethyl acetal (17). The methanol which was formed during the reaction was removed continuously from the reaction solution by distillation. After the reaction solution had cooled down, it was extracted with heptane and the solvent was evaporated. This resulted in 303 g of crude product 22 (yield 70%), which was reacted without any further purification.
Aufarbeitung
- customwas removed continuously from the reaction solution by distillation
- temperatureAfter the reaction solution had cooled down
- extractionit was extracted with heptane
- customthe solvent was evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-61ae3168daba4471836d74f929444277
- Quelldatensatz
- uspto-grants-2014_07
- Patentnummer
- US08778955B2
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