QUINOLINE, 2-(9,9-DIMETHYL-9H-FLUOREN-2-YL)- synthesis

Yield:889750-37-2 82%

Reaction Conditions:

with sodium carbonate;tetrakis(triphenylphosphine) palladium⁽⁰⁾ in ethanol;water;toluene; for 6 h;Heating / reflux;

Steps:

1

4.7 g (20 mmole) of Compound (Bl), 3.3 g (20 mmole) of Compound (B2), 0.22 g (0.17 mmole) of tetrakistriphenylphosphine palladium, 20 ml of a 2M aqueous solution of sodium carbonate, 10 ml of ethanol, and 20 ml of toluene were fed into a 200-ml round-bottomed flask, and the whole was stirred for 6 hours under hot reflux in a stream of nitrogen. The reaction solution was poured into 100 ml of cold water, and 50 ml of toluene were added to the mixture to carry out liquid separation for separating an organic layer, followed by concentration. The resultant solid material was purified by means of a silica gel column (eluent: toluene), and the purified product was recrystallized with hexane to yield 5.3 g of a crystal of Compound (B3) (82% yield) .

References:

WO2006/59758,2006,A1 Location in patent:Page/Page column 21-22