Carbon Dioxide → HCID 13772985, compound

Participants

Reaction Steps

661.4 ml (1.084M) of a 15% solution of n-butyl-lithium in hexane are added at 0°, over a period of 20 minutes and under a nitrogen atmosphere, to a solution of 97 g (0.328M) of 9-ethylamino-3,4-dimethoxy-6-methyl-phenanthrene in 1000 ml anhydrous tetrahydrofuran; the reaction mixture becomes dark red. After stirring for 30 minutes at 0°, the mixture is transferred in portions with a teflon tube with nitrogen pressure at -50° onto a mixture of 500 g sodium sulfate and 500 g dry ice in 1500 ml tetrahydrofuran. After the temperature of the mixture has reached room temperature, the mixture is poured onto water/ice, extracted three times with methylene chloride. The combined organic phases are dried over sodium sulfate and evaporated to give the title compound. M.pt. 158°-160° (decomp.) after crystallisation from ether/petroleum ether.

Provenance & Evidence