Potassium Carbonate → HCID 66871015, compound

Participants

Reaction Conditions

Reaction Steps

A well-stirred suspension of 35.5 g (50 mmol) of 4,4′-bis(diphenylamino)-1,1′-dimethoxy-9,9′-spirobifluorene, 18.1 g (100 mmol) of 1-phenyl-5-chlorotetrazole and 27.6 g (200 mmol) of K2CO3 is heated under reflux for 18 h in 250 ml of acetone. After cooling, the precipitated solid is filtered off with suction and dried. The solid is dissolved in 200 ml of toluene, 6 g of Pd/C (5%) are added, and the mixture is stirred at 40° C. for 8 h under a hydrogen atmosphere. After removal of the solvent, the residue is washed three times with 50 ml of ethanol:water (1:1, v:v) and three times with 100 ml of ethanol and subsequently recrystallised three times from DMF (about 10 ml/g). Yield: 21.1 g (32.43 mmol), 65.0%, purity: 99.9% (HPLC).

Provenance & Evidence