Chloromethyl ethyl ether → HCID 23116094、化合物
反応式
[CH:1]([N:4]1[CH2:8][CH2:7][CH2:6][CH2:5]1)([CH3:3])[CH3:2].[CH2:9]([O:11][CH2:12][Cl:13])[CH3:10]>CC(=O)CC>[Cl-:13].[CH2:9]([O:11][CH2:12][N+:4]1([CH:1]([CH3:3])[CH3:2])[CH2:8][CH2:7][CH2:6][CH2:5]1)[CH3:10]参加物
4
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.