Multigram-Scale Synthesis of Third-Generation Buchwald Precatalysts Containing Xphos
Sotnik, Svitlana O., et al. Molecules, 2021, 26(12), 3507.
XPhos Pd G3 is a catalyst used in organic synthesis, particularly in cross-coupling reactions such as Suzuki-Miyaura and Buchwald-Hartwig reactions. It is a highly efficient and air-stable catalyst that contains palladium as its active metal. XPhos Pd G3 is known for its ability to promote reactions under milder conditions and provide excellent yields and selectivity.
Synthesis of XPhos Pd G3
· A two-necked 2 L round bottom Schlenk flask equipped was charged with [Pd(ABP)(OMs)]2 (53.6 g, 64 mmol, 0.5 eq.) and XPhos (61.5 g, 129 mmol, 1 eq.). The flask was capped, three times evacuated and backfilled with argon.
· Anhydrous and deoxygenated tetrahydrofuran (1.4 L) were added in the flask under argon counterflow. The reaction mixture was stirred at room temperature for 1.5 h and then it was filtered under argon atmosphere.
· About 1.2 L of the filtrate was evaporated under vacuum via a rotor evaporator. Deoxygenated hexane (1.2 L) was added to the dark brown residue and the formation of a beige precipitate was observed.
· The flask was placed in an ultrasonic bath and sonicated for 20 min. A beige precipitate was filtered, washed with hexane (3× 250 mL) and dried under vacuum at 50 °C for 1 h to obtain 92.0 g of XPhos Pd G3.
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