Abstract: Tetrakis (trifluoromethy1)-1, 4-diphosphabenzene (3b), the first example of diphosphabenzenes, was synthesized by the thermolysis of 2, 3, 5, 6.7, 8-hexakis (trifluoromethyl)-7-methoxy-1, 4-diphosphabicycl0 [2.2. 2] octa-2, 5-diene (6), which was obtained by addition of methanol to hexakis (trifluoromethyl)-1, 4-diphosphabarrelene (5) in the presence of rhodium trichloride or some other catalysts. The compound 3b seems to ...