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Reaction Procedure of Appel Reaction & Workup

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Org. Synth.   1974 ,  54 , 63 DOI: 10.15227/orgsyn.054.0063 Example 1:- GERANYL CHLORIDE [ 2,6-Octadiene, 1-chloro-3,7-dimethyl-,  (E) - ] Submitted by Jose G. Calzada and John Hooz 1 . Checked by K.-K. Chan, A. Specian, and A. Brossi. 1. Procedure A dry,  300-ml., three-necked flask  is equipped with a  magnetic stirring bar  and  reflux condenser  (to which is attached a  Drierite-filled drying tube ) and charged with  90 ml. of  carbon tetrachloride   (Note 1)  and  15.42 g. of  geraniol (0.1001 mole)   (Note 2) . To this solution is added  34.09 g. (0.1301 mole) of  triphenylphosphine   (Note 3) , and the stirred reaction mixture is heated under reflux for 1 hour. This mixture is allowed to cool to room temperature; dry  pentane  is added (100 ml.) , and stirring is continued for an additional 5 minutes. The  triphenylphosphine oxide ...