Hydrochloric Acid → N,N-Diethylacrylamide

温度

140 °C

7.2 parts 30% methanolic Na-methylate solution are added to 36.5 parts diethylamine. 77 parts 2-carbomethoxy-7-oxabicyclo(2,2,1)hept-5-ene are added drop-wise at 40° C. The reaction medium is then stirred for 15 hours at this temperature and neutralised with 4 parts concentrated hydrochloric acid. 100 parts methylene chloride and 50 parts water are added, the organic phase separated off, and the aqueous phase extracted 3 times with 25 parts methylene chloride in each instance. The combined organic phases are reduced in a rotary evaporator at a bath temperature of 90° C. and under a vacuum of 20 Torr. The residue is heated under a vacuum of 20 Torr to 110° to 120° C. (bath temperature 140° C.). On conclusion of the furane separation, the sedimentation temperature increases and the product distills over at the now lowered pressure. 21 parts N,N-diethylacrylamide with a boiling point of 55° C. at 1 Torr are obtained.

1. customthe organic phase separated off
2. extractionthe aqueous phase extracted 3 times with 25 parts methylene chloride in each instance
3. customThe combined organic phases are reduced in a rotary evaporator at a bath temperature of 90° C.
4. customOn conclusion of the furane separation
5. temperaturethe sedimentation temperature increases
6. distillationthe product distills over at the now lowered pressure

ORDレコード

ord-26fbb501dc83464bbb6d1b5292d80de1

出典データセット

uspto-grants-1986_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04605740