[摘要]:Phosphorus(V) chloride was sequentially displaced by catechol N,O-bis(trimethylsilyl)amino acids and phenol (Method A) or catechol, phenol and N,O-bis(trimethylsilyl)amino acids (Method B) leading to a high yield synthesis of 2-phenoxy-2,7(5)-spiro[1,3,2-benzodioxaphosphole-2,2'-1,3,2-oxazophosph olan]-5'-ones under mild conditions. The products were characterized by H-1, C-13, H-1-H-1 COSY, H-1-C-13 COSY and held desorption mass spectrometry.