Compound 1a

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InChIKey ARICQYJMIOTXCN-UHFFFAOYSA-K

Compound data: CIF

Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.

A mixture of 2,6-bis(di-tert-butylphosphinomethyl)pyridine (2.00 g, 5.06 mmol) and [MoCl₃(thf)₃] (2.01 g, 4.80 mmol) in THF (60 mL) was stirred at 50 °C for 18 h. The resultant orange suspension was concentrated under reduced pressure, and the residue was recrystallized from CH₂Cl₂ (50 mL)−hexane (100 mL) to give orange-brown crystals of 1a·0.75CH₂Cl₂, which were collected by filtration and washed with Et₂O (15 mL × 3) and dried in vacuo to afford 1a as an orange-brown solid (2.71 g, 4.53 mmol, 94% yield). Anal Calcd for C₂₃H₄₃Cl₃MoNP₂: C, 46.21; H, 7.25; N, 2.34. Found: C, 46.01; H, 7.25; N, 2.22.