反应详情

A 12-l. three-necked flask, equippedewith a thermometer, mechanical stirrer and a reflux condenser was charged under an atmosphere of nitrogen with 746 g (6.26 moles) of nitroacetic acid methylester, 1392 g (9.4 moles) of triethyl orthoformate and 1.92 l of acetic anhydride. The mixture was stirred and heated at reflux for 23 hours. The volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C, then at aspirator; vacuum and finally at 0.17 mmHg, (pot temperature up to 70°), leaving 926 g (84%) of crude alpha-nitro-beta-ethoxyacrylic acid methylester as an orange oil.

1. temperatureheated
2. temperatureat reflux for 23 hours
3. distillationThe volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C