反应详情

温度

120 °C

A mixture of magnesium methyl carbonate and dimethylformamide (300 g of a 2.0mM/g solution) is heated in a 120° C. oil bath with stirring under carbon dioxide flushing for 1/2 hour. To this mixture is added 33.8 g (0.100 mole) of 5-(tetradecyloxy)-2-thienyl methyl ketone, and the oil bath temperature is raised to 130° C. to 150° C. Dry nitrogen is flushed through the mixture for 5 hours. The mixture is allowed to cool at room temperature under carbon dioxide flushing after which it is poured slowly into 3 liters of concentrated HCl-ice (1:1) with vigorous stirring. When the evolution of gas is complete, the precipitate is collected and washed with cold water, then dried to give 5-tetradecyloxythen-2-oylacetic acid.

1. temperaturethe oil bath temperature is raised to 130° C. to 150° C
2. customDry nitrogen is flushed through the mixture for 5 hours
3. temperatureto cool at room temperature under carbon dioxide flushing after which it
4. additionis poured slowly into 3 liters of concentrated HCl-ice (1:1) with vigorous stirring
5. customthe precipitate is collected
6. washwashed with cold water
7. customdried