反应详情

温度

180 °C

The reaction for the selective methylation is carried out placing into a 250 ml (φi =45 mm) stainless steel autoclave a mixture of (3-methoxycarbonylphenyl)acetonitrile (10 g, 96% purity), dimethyl carbonate (86 ml) and K2CO3 (12 g), in the 1:18:2 molar ratio. Air is replaced by a N2 stream; then the mixture is heated at a temperature of 180° C., with stirring. During the reaction, which is completed within 6 hours, the pressure raises from 7 bars, reached at the working temperature, to about 12 bars after 5 hours of isothermal heating. After cooling K2CO3 is filtered off, DMC is recovered and the residue is distilled (b.p. 0.078=109°-110° C.) to obtain 8.3 g of 2-(3-methoxycarbonyl-phenyl)propionitrile which is 99,5% pure (78% yield) (>99% selectivity in monomethylation).

1. customThe reaction for the selective methylation
2. customDuring the reaction, which
3. temperaturethe pressure raises from 7 bars
4. waitreached at the working temperature, to about 12 bars after 5 hours of isothermal heating
5. filtrationis filtered off
6. customDMC is recovered
7. distillationthe residue is distilled (b.p. 0.078=109°-110° C.)