反应详情

温度

160 °C

A mixture of 63C (6.15 g, 0.015 mol), sodium trifluoroacetate (9.52 g, 0.07 mol), copper-(I)iodide (13.37 g, 0.07 mol) and 1-N-methyl-2-pyrrolidinone (100 ml) is heated to 160° C. for 118 hours. The reaction mixture is cooled to room temperature and diluted with ether and water. The organic phase is separated and concentrated and the residue is purified by column chromatography (petrol ether:ethyl acetate, 95:5 v/v) yielding the pure product as white crystals, 1.3 g, (22%) having a melting point of 95-96° C.

1. temperatureThe reaction mixture is cooled to room temperature
2. customThe organic phase is separated
3. concentrationconcentrated
4. customthe residue is purified by column chromatography (petrol ether:ethyl acetate, 95:5 v/v)