Cyclohexylphosphonic dichloride

Cyclohexylphosphonic dichloride 159 Oxygen is passed into a vigorously stirred mixture of cyclohexane (2 moles) and phosphorus trichloride (1 mole) under a reflux condenser. The mixture heats up immediately. The stirrer should be adjusted to throw as much liquid as possible up into the gas space. The reaction is ended when the temperature, which has been held between 20° and 30° by external cooling, falls materially. With an oxygen stream of 6-8 1/h this usually occurs after about 2 h. The unchanged components are distilled off and the residue is fractionated in a vacuum. The fraction distilling at 140-150°/15 mm solidifies rapidly and is redistilled in a vacuum this affords 60-70% (calculated on PC13 60-70 g) of the dichloride, m.p. 41°. 

Chlorophenylphosphorodichloridate 12 Cyclohexylphosphonic dichloride 12 n-Butylphosphorodichloridate 1 Phenylphosphonothioic dichloride 0 Phenylphosphorodichloridate 12 Phenylphosphonic dichloride 79... 

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