反应详情

温度

25 °C

182.21 g (1.4 mol) of ethyl acetoacetate and 169.98 g (1.4 mol) of triethylamine were dissolved in a mixed solvent of 182 mL of tetrahydrofuran and 1.64 L of hexane under nitrogen atmosphere. To this solution, 167.3 g (1.54 mol) of trimethylsilyl chloride was added dropwise at a temperature of 21 to 45° C., and then the solution was stirred at 25° C. for 3 hours. The reaction mixture was cooled to 10° C., the reaction was ceased by adding 547 mL of water thereto and an organic layer was separated. The organic layer was washed two times with 273 mL of water, dried over 54.7 g of anhydrous magnesium sulfate, and then filtered. The solvent was evaporated to obtain 301.3 g (crude yield 106.4%) of 3-(trimethylsilyloxy) but-2-enoic acid ethyl ester.

1. temperatureThe reaction mixture was cooled to 10° C.
2. customan organic layer was separated
3. washThe organic layer was washed two times with 273 mL of water
4. dry with materialdried over 54.7 g of anhydrous magnesium sulfate
5. filtrationfiltered
6. customThe solvent was evaporated