Reaktionsgleichung
[C:1]([O:5][CH2:6]C)(=[O:4])[CH:2]=[CH2:3].[CH2:8]([N:15]([CH2:21]OC)[CH2:16][Si](C)(C)C)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.FC(F)(F)C(O)=O>ClCCl>[CH2:8]([N:15]1[CH2:21][CH2:3][CH:2]([C:1]([O:5][CH3:6])=[O:4])[CH2:16]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
Ethyl acrylate (86 g, 1.0 mole) in dichloromethane (2 L) was cooled to 0° C. and treated with N-benzyl-N-(methoxymethyl)-N-[(trimethylsilyl)methyl]amine (compound D17 of EP 0363085) (300 g, 80% pure by 1H NMR, 1 mole) with stirring over a period of 10 min whilst maintaining the temperature between -5° C. and 0° C. A solution of trifluoroacetic acid in dichloromethane (100 ml, 1 molar) was added at such a rate that the temperature did not rise above 5° C. and the reaction allowed to warm to room temperature overnight. The solution was then washed with saturated aqueous potassium carbonate solution, dried over sodium sulphate and concentrated in vacuo to a gum. The glum was distilled in vacuo to afford the title compound. (D4) as a single main fraction. Bpt 150°-160° at 8 mm (232 g, 100%).
Aufarbeitung
- temperaturewhilst maintaining the temperature between -5° C. and 0° C
- customdid not rise above 5° C.
- washThe solution was then washed with saturated aqueous potassium carbonate solution
- dry with materialdried over sodium sulphate
- concentrationconcentrated in vacuo to a gum
- distillationThe glum was distilled in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-c7013366f2ce4f4ea80eb3c86ea0cf70
- Quelldatensatz
- uspto-grants-1995_11
- Patentnummer
- US05470859
Verknüpfte Notizen
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