The reduction of benzyl-containing phosphonium compounds with lithium aluminum hydride has been used for the synthesis of two unsymmetrical tertiary phosphines. Thus et hylmethylphenylphosphine was prepared from dichlorophenylphosphine in an over-all yield of 5954. Similarly, ethylmethylpentylphosphine was prepared from dichloromethylphosphine in an over-all yield of 507,.