The Preparation of Optically Active Hydrazines I the Preparation of Dl P Trime

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The Preparation of Optically Active Hydrazines I the Preparation of Dl P Trime
Charles H Milligan
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The next step was to reduce the un- saturated hydrocarbon to the saturated one. One hundred and twenty-five g. Of the crude trimethyl-phenyl^ethylene (boiling range 175-200) was treated, in a flask fitted with a wide reflux condenser, with 30 g. Of red phosphorus and 50 cc. Of a saturated solution of hydrogen iodide. The re- action mixture was heated to boiling and iodine added carefully in small portions through the condenser until fumes due to escaping hydrogen iodide were visible at the top ...of the condenser. The mixture was kept boiling until the color due to iodine in the hydrocarbon disappeared. The reaction mix- ture was now subjected to distillation. The distillate formed 2 layers of almost equal volume of which the lower was hydriodic acid, the upper almost pure hydrocarbon. The layers were separated, the hydriodic acid returned to the reaction flask, and again distilled. This process was re- peated as long as any hydrocarbon separated in the distillate.
The hydrocarbon was then washed with water and dil.


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