Hydrotris 3,5-Dimethyl-l-pyrazolyl borato oxomolybdenum V ethyleneglycolate LMoO Eth-Gly

4-CATECHOLATO[HYDROTRIS(3,5-DIMETHYL-l-PYRAZOLYL)BORATO]OXOMOLYBDENUM(V) - 

Attachment of the molybdenum center to the pendant catecholato group is described in this section and Section H. 

Amounts of 3,4-OH-TTP (0.5 g, 0.7 mmol) and LMo O(eth-gly) (0.7 g, 1.5 mmol) are placed in an evacuated Schlenk flask (250 mL). Degassed dry toluene (100 mL) is added and the mixture is stirred at 70°C. Heating the solution to 100°C lowers the yield. Heating is continued until the reaction is complete as evidenced by TLC the organic solvent is removed under vacuum. Dichloromethane/toluene (1 1) (25 mL) is added to yield a purple-brown solution. The solution is purified by chromatography on a silica gel column (3x30 cm) with dichloromethane/toluene (1 1) as eluant. The solvent is removed under vacuum. Recrystallization from dichloromethane-heptane gives dark purple microcrystals. Yield 0.65 g (82%). 

This synthesis follows the procedure described above for 3,4-Mo-TTP but utilizing the 2,3-OH-TTP porphyrin. Yield 0.70 g (88%). 

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