Potassium Carbonate → HCID 54443158, compound

Participants

Reaction Steps

Isopropyl 3-(3,5-dimethoxy-4-hydroxyphenyl)-2-(dimethoxy-phosphinyl)propenoate (4 g; 0.01 mol; Table 1, No. 10) was dissolved in 60 ml of acetonitrile, and potassium carbonate (4.45 g; 0.032 mol) and 4-methoxybenzyl chloride (1.4 ml; 0.011 mol) were added and the mixture was initially stirred at room temperature for 8 hours. To complete the reaction, 0.7 ml of 4-methoxybenzyl chloride was added, followed by stirring for 4 hours, after which the result of a thin-layer chromatography showed that the reaction was complete. The filtrate after removal of potassium carbonate by filtration was evaporated to dryness under reduced pressure, and the residue is chromatographed (SiO2 ; CH2CI2 : AcOEt=8:2). This resulted in a slowly crystallizing oil which, on solidification, had a melting point of 68° to 69° C.

Provenance & Evidence