Sodium Carbonate → HCID 86682756, compound

Participants

Reaction Steps

A mixture of 17.0 g (50 mmol) of 10-bromo-3,5,8-trimethylindazolo[2,3-a]-quinoline (Example 86), 19.8 g (65 mmol) of 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzo[h]quinoline, 225 mg (1 mmol) of palladium(II) acetate, 1.8 g (6 mmol) of tri-o-tolylphosphine, 10.6 g (100 mmol) of sodium carbonate, 200 ml of toluene, 50 ml of dioxane and 300 ml of water is heated under reflux for 16 h. After cooling, the organic phase is separated off, washed twice with 300 ml of water, dried over magnesium sulfate, the organic phase is evaporated to dryness in vacuo, and the residue is recrystallised from toluene/ethanol. 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 270° C.). Yield: 15.8 g (36 mmol), 72%, purity: about 99.5% (NMR).

Provenance & Evidence