Chloromethyl ethyl ether → HCID 23116094, compound

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.

1. temperatureThe mixture was thereafter heated to a gradually elevated temperature
2. customwhereby the reaction was terminated
3. temperatureThe reaction mixture was cooled to 5° C.
4. filtrationthe resulting solids were filtered off in nitrogen
5. washThe filter cake was washed with 200 ml of 2-butanone
6. washfurther washed with 200 ml of acetone
7. customdried in a vacuum

ORD record

ord-f4819e69156d4d829fe4a5907091e3f1

Source dataset

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08366956B2