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A 12-1. three-necked flask, equipped with 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. customthree-necked flask, equipped with a thermometer, mechanical stirrer and a reflux condenser
2. temperatureheated
3. temperatureat reflux for 23 hours
4. distillationThe volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C.