Water → Methyl Acrylate

温度

20 °C

1290 g (15 Mol) methylacrylate is prepared and 67.5 g (0.5 Mol) AlCl3 added thereto and dissolved with stirring. At 20° to 25° C., 1050 g (15.4 Mol) furane is added drop-wise during cooling. The temperature is maintained at 20° C. until the exothermic reaction is finished, after which stirring is continued for a further hour at 20° C. and then for 3 hours at 10° C. 300 g water is then added, the organic phase separated, and the unconverted furane and the methylacrylate distilled off under a pressure of 10 Torr and at a bath temperature of 60° C. in a rotary evaporator. Finally, the vacuum is lowered to 1 Torr and further volatile components drawn off. The crude product is passed to a thin-film evaporator under a vacuum of 1 Torr and a thermostatically controlled temperature of 95° C. A distillation temperature of approximately 70° C. is used. The 2-carbomethoxy-7-oxabicyclo(2,2,1)hept-5-ene is obtained in a yield of 1060 g (45.9% theoretical).

1. dissolutiondissolved
2. temperatureduring cooling
3. stirringafter which stirring
4. waitis continued for a further hour at 20° C.
5. customthe organic phase separated
6. distillationthe unconverted furane and the methylacrylate distilled off under a pressure of 10 Torr and at a bath temperature of 60° C.
7. customin a rotary evaporator
8. customThe crude product is passed to a thin-film evaporator under a vacuum of 1 Torr
9. customa thermostatically controlled temperature of 95° C
10. customA distillation temperature of approximately 70° C.

ORDレコード

ord-a289d304ea744587904277b0d0f30caa

出典データセット

uspto-grants-1985_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04555581