Improved Synthesis of Asymmetrical Substituted 1H-1,2,4-Diazaphospholes

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• The formation of two additional symmetric 1H-3,5-substituted 1,2,4-diazaphospholes H[3,5-R1R1dp] and H[3,5-R2R2dp] indicates moderate yields of 3 due to the presence of the two symmetric 1,3-bis(amino)-2-phosphaallyl chlorides in the system. The 31P NMR data of the unsymmetrical phosphaallylic salts are not reliable for publication due to incomplete separation.
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• Note: The quality of the crystallographic data of tetrameric 3f is not warranted for publication due to the disorder of tBu group, but the structural connections are reliable: C10H13N2OP, Mr = 208.19, tetragonal, space group I4(1)/a, a = 19.6212(4) Å, b = 19.6212(4) Å, c = 11.9224(5) Å, α = β = γ = 90°.
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