Synthesis and Crystal Structure of 2-Ethoxy-spiro[2H-1, 4,2-benzoxazaphosphorine-3(4H), 1'-Cycl

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The title compound 2-ethoxy-spiro[2H-1,4,2-benzoxazaphosphorine-3(4H),1'-cyc- loheptane] 2-oxide (C15H22NO3P) was synthesized by the Mannich-type reaction of o-amino-phenol with ethyl dichlorophosphinite and cycloheptanone, and structurally characterized by single-crystal X-ray diffraction analysis. It crystallizes in orthorhombic, space group P212121 with a = 8.9840(12), b = 9.2978(12), c = 37.205(5)(A), V = 3107.8(7)(A)3, Z = 8, Mr = 295.31, Dc = 1.262 g/cm3, F(000) = 1264, μ = 0.184 mm-1, S = 1.026, the final R = 0.0502 and wR = 0.1017 for 3849 observed reflections with I > 2σ(I) and 378 variable parameters. The structure exhibits that the six-membered phosphorus heterocycle is in the envelope conformation.
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