反应 #1725395
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06114391
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of triphenylphosphine (0.117 moles, 30.8 g) in acetone (200 ml) is added under a nitrogen stream at r.t. with Cu (I) bis-(triphenyl-phosphine)-tetrahydroborate (0.067 moles, 40.69 g), then 3-(4-methylphenyl)propanoyl chloride (0.055 moles, 10 g) dissolved in acetone (85 ml) is dropped in 45'. The mixture is stirred at r.t. under nitrogen for 1 h. The precipitated solid is filtered, washing with acetone and the filtrate is evaporated under vacuum. The residue is dissolved in chloroform (340 ml), added with cuprous chloride (0.135 moles, 13.38 g) and stirred under nitrogen stream for 1 h at r.t. The mixture is filtered through celite, the filtrate is evaporated to dryness and the resulting residue is taken up into ethyl ether and petroleum ether, filtered and evaporated under vacuum to obtain an oil. Yield: 6.7 g (83%) is dropped in 45' The precipitated solid is filtered washing with acetone the filtrate is evaporated under vacuum The residue is dissolved in chloroform (340 ml) stirred under nitrogen stream for 1 h at r.t The mixture is filtered through celite the filtrate is evaporated to dryness filtered evaporated under vacuum to obtain an oil
来源 ID: ord-6809b637859049dc9b3ad624c7f55e31