反应详情

温度

180 °C

A mixture of the bromide (0.240 g) of example 176, Cu(I)CN (0.060 g) and N-Methyl pyrrolidinone (5 ml) was heated at 180° C. for 16 h. The cooled reaction mixture was diluted with ethyl acetate and passed through kiesselguhr, washing with ethyl acetate. The filtrate was washed with water, dried (sodium sulfate) and solvent removed at reduced pressure. The residue was column chromatographed (silica gel, 20-50% ethyl acetate-pentane) to give the title compound as a pale yellow gum (0.101 g

1. customThe cooled reaction mixture
2. washwashing with ethyl acetate
3. washThe filtrate was washed with water
4. dry with materialdried (sodium sulfate) and solvent
5. customremoved at reduced pressure
6. customchromatographed (silica gel, 20-50% ethyl acetate-pentane)