反应详情

温度

55 °C

0,35 g (0,5 mmol) Pd[TPP]2Cl2 and 0.12 g (=0.6 mmol) of copper(I) iodide and, with stirring in the course of a few minutes, 10.7 g (=0.13 mmol) of 1-methyl-3-butyn-1-ol are added to a solution of 21.3 g (=0.1 mol) of 4-bromophenylacetone in 250 ml of triethylamine. The mixture is warmed to 55° C. and the temperature is allowed slowly to rise to 80° C. during the course of 4 hours. After cooling, the mixture is filtered and the filtrate is concentrated. The oil which remains is chromatographed on silica gel. 17.4 g (90.3% of theory) of 4-(3-hydroxy-3-methyl-1-butynyl)phenylacetone are obtained; m.p. 67-69° C.

1. customto rise to 80° C. during the course of 4 hours
2. temperatureAfter cooling
3. filtrationthe mixture is filtered
4. concentrationthe filtrate is concentrated
5. customThe oil which remains is chromatographed on silica gel