反应详情

A mixture consisting of 28.7 g (0.10 mol) of 2,4-di-tert-butyl-6-cyclohexen-1-yl-phenol (compound 102, Example 1b) and 17.5 ml (0.20 mol) of phosphorus trichloride is refluxed under nitrogen for 5 hours. Excess phosphorus trichloride is removed by distillation and the residue is then distilled under vacuum at 165-167° C./0.01 mbar, giving 30.8 g (88%) of 6,8-di-tert-butyl-10-chloro-2,3,4,10-tetrahydro-l H-9-oxa-10-phosphaphenanthrene, a colourless thick liquid which slowly crystallises when standing; 31P--NMR (CDCl3): δ=130.5 ppm (s); 1H--NMR (CDCl3): δ(ppm): 1.34 (s, 9H, (CH3)3C--), 1.44 (s, 9H, (CH3)3C--), (compound (202), Table 2).

1. temperatureis refluxed under nitrogen for 5 hours
2. customExcess phosphorus trichloride is removed by distillation
3. distillationthe residue is then distilled under vacuum at 165-167° C./0.01 mbar