反応 #470375
ord-9209a896dfa1435f880b571e2d41bd2d
反応方程式
反応条件
後処理
- 1温度The mixture was thereafter heated to a gradually elevated temperature
- 2その他whereby the reaction was terminated
- 3温度The reaction mixture was cooled to 5° C.
- 4ろ過the resulting solids were filtered off in nitrogen
- 5洗浄The filter cake was washed with 200 ml of 2-butanone
- 6その他dried in a vacuum
実験手順
A 40.00 g quantity of N-isopropylpyrrolidine was dissolved in 361 g of dehydrated 2-butanone (reagent, product of Wako Pure Chemical Ind. Ltd.), followed by replacement with nitrogen. To the solution was added dropwise 28.76 g of chloromethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd. as purified by distillation) at 5° C. over a period of 0.5 hour. The mixture was thereafter heated to a gradually elevated temperature and stirred at room temperature for 10 hours, whereby the reaction was terminated. The reaction mixture was cooled to 5° C., and the resulting solids were filtered off in nitrogen. The filter cake was washed with 200 ml of 2-butanone and thereafter dried in a vacuum, giving 66.40 g of the desired product.