Triphenylphosphine → HCID 66665890, compound

Participants

Reaction Steps

A solution of 15.3 g (50 mmol) of 2-(2-nitrophenyl)-4-tert-butylquinoline and 34.1 g (130 mmol) of triphenylphosphine in 150 ml of o-dichlorobenzene is heated under reflux for 12 h. After cooling, the solvent is removed in vacuo, the residue is recrystallised twice from ethyl acetate and then chromatographed on silica gel (DCM:heptane 3:1, v:v+0.2% of triethylamine). The solid obtained in this way is freed from readily volatile and non-volatile secondary components by fractional sublimation (p about 1×10−5 mbar, T about 180° C.). Yield: 8.8 g (32 mmol), 64%, purity: about 99.5% (NMR).

Provenance & Evidence