反応 #470376

反応方程式

N-isopropylpyrrolidine

chloromethyl ethyl ether

→

desired product

N-Ethoxymethyl-N-Isopropylpyrrolidinium Chloride

溶媒

2-butanone

反応条件

後処理

1. 1
   温度The mixture was thereafter heated to a gradually elevated temperature
2. 2
   その他whereby the reaction was terminated
3. 3
   温度The reaction mixture was cooled to 5° C.
4. 4
   ろ過the resulting solids were filtered off in nitrogen
5. 5
   洗浄The filter cake was washed with 200 ml of 2-butanone
6. 6
   洗浄further washed with 200 ml of acetone
7. 7
   その他dried in a vacuum

実験手順

A 40.09 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 33.54 g of chloromethyl ethyl 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, further washed with 200 ml of acetone and dried in a vacuum, giving 55.72 g of the desired product.

出典