反应详情

Distilled di-n-butyl ether (2500 ml) and solid sodium metal (230 g, 10.0 moles) were placed in a 22 L round bottom flask. The flask was equipped as in the above Comparative Example C-1. The solution of the sodium phosphide salt was made by carefully adding diphenylphosphinous chloride (1100 g, 5.0 moles) to the refluxing solvent-sodium slurry as described in the previous example. Stirring and reflux was continued for 2 hours after addition of the diphenylphosphinous chloride was complete. The reaction mixture was cooled with further stirring to about 45° C. n-Hexyl chloride (603 g, 5 moles) was added over a 30 minute period. Stirring was continued for 30 minutes after this addition was complete. Water (2500 ml) was added with stirring and the inorganic salts dissolved. Stirring was stopped and the lower water layer drained off and discarded. The upper organic layer was concentrated under vacuum giving crude n-hexyldiphenylphosphine (1190 g) of about 87 percent yield based on diphenylphosphinous chloride. This material was found to be about 20 percent n-hexyldiphenylphosphine oxide by GLC analysis.

1. customwere placed in a 22 L round bottom flask
2. temperaturereflux
3. temperatureThe reaction mixture was cooled
4. additionwas added over a 30 minute period
5. stirringStirring
6. waitwas continued for 30 minutes
7. additionafter this addition
8. stirringwith stirring
9. dissolutionthe inorganic salts dissolved
10. stirringStirring
11. concentrationThe upper organic layer was concentrated under vacuum