反应详情

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%).

1. temperaturewhilst maintaining the temperature between -5° C. and 0° C
2. customdid not rise above 5° C.
3. washThe solution was then washed with saturated aqueous potassium carbonate solution
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated in vacuo to a gum
6. distillationThe glum was distilled in vacuo