Tris(1,1-dimethylethyl)phosphine → HCID 66797973, compound

Participants

Reaction Steps

15.8 g (47 mmol) of (3′-bromobiphenyl-3-yl)phenylmethanone, 13.36 g (47 mmol) of 10,10-dimethyl-10,12-dihydro-3,12-diazaindeno[2,1-b]fluorene and 29.2 g of Rb2CO3 are suspended in 250 ml of p-xylene. 0.95 g (4.2 mmol) of Pd(OAc)2 and 12.6 ml of a 1 M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 24 h. After cooling, the organic phase is separated off, washed three times with 150 ml of water and subsequently evaporated to dryness. The residue is extracted with hot toluene, recrystallised three times from toluene and finally sublimed in a high vacuum, giving 14.2 g (26.3 mmol), corresponding to 56% of theory. The purity is 99.9%.

Provenance & Evidence