Abstract
Abstract We report the first examples of phosphorus-containing derivatives of a disulphonylamine in which the phosphorus atom is bound directly to the amine nitrogen. Ph2P[sbnd]N(SO2Me)2 (1), 2-dimesylamino-1,3,2-benzodioxaphosphole (2a) and P[N(SO2Me)2]3 (3) are obtained by elimination of Me3SiCl from the corresponding phosphorus chlorides and stoichiometric amounts of Me3SiN(SO2Me)2. 2a is also formed by silver salt metathesis between the 2-chlorophosphole and AgN(SO2Me)2. Cleavage of R2P(S[sbnd]P(S)R2 with ClN(SO2Me)2 affords R2P(S)[sbnd]N(SO2Me)2 with R = Me (4a) and Et (4b), the co-product being R2P(S)Cl. 2a reacts with oxygen to form 2-dimesylamino-2-oxo-1,3,2-benzodioxaphosphole (2b). 1 crystallizes in the monoclinic space group P21/n with a = 1461.8(5), b = 732.2 (3), c = 1511.0(4) pm, β = 97.59(3)°, V = 1.6030 nm,3 Z = 4. The crystallographic data for 2a are: Triclinic, space group P1, a = 561.5(2), b = 886.8(2), c = 1272.9(4) pm, α = 73.99(3), β = 83.56(3), γ = 81.54(3)°, V = 0.6009 nm,3 Z = 2. ...
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