反应详情

To 12.6 g. of magnesium turnings was gradually added a solution containing 96 g. (0.50 mole) of p-chlorobromobenzene and 1.80 cc. tetrahydrofuran. The reaction mixture was stirred and maintained under a nitrogen atmosphere during the addition, following which the contents of the vessel were heated to reflux temperature for two hours. When the reaction mixture had cooled, a solution of methyldichlorophosphine (29.3 g., 0.25 mole) in 25 cc. tetrahydrofuran was gradually added. Following completion of this addition the reaction mixture was heated to reflux temperature for two hours. When the mixture had cooled it was slowly poured into 500 cc. of cold water and then acidified to a pH of 5 using aqueous hydrochloric acid. The resultant aqueous solution was extracted using chloroform. The organic layer was then dried over anhydrous magnesium sulfate and the chloroform removed under reduced pressure. The residue remaining followng removal of the chloroform weighed 64 g. and was distilled, the fraction boiling at between 155 and 160 under a pressure of 0.5 mm Hg being collected. This distillate converted to a white solid upon cooling. The solid material weighed 34 g. and exhibited the following analysis:

1. additioncontaining 96 g
2. temperaturemaintained under a nitrogen atmosphere during the addition
3. temperaturewere heated
4. temperatureto reflux temperature for two hours
5. temperatureWhen the reaction mixture had cooled
6. additioncompletion of this addition the reaction mixture
7. temperaturewas heated
8. temperatureto reflux temperature for two hours
9. temperatureWhen the mixture had cooled it
10. additionwas slowly poured into 500 cc
11. extractionThe resultant aqueous solution was extracted
12. dry with materialThe organic layer was then dried over anhydrous magnesium sulfate
13. customthe chloroform removed under reduced pressure
14. customremoval of the chloroform
15. distillationand was distilled
16. custombeing collected
17. temperatureupon cooling