Chloroform → Hexafluorophosphate

Participants

Reaction Conditions

Reaction Steps

In a reactor were put 24 mmol of an indolenine quaternary salt (bromide), 30 mmol of ferrocene carbaldehyde, and 26 g of chloroform, and the mixture was stirred at 85° C. for 9 hours. To the reaction mixture were added 30 mmol of sodium perchlorate or potassium hexafluorophosphate and 30 g of water, and the mixture was stirred at 60° C. for 1 hour, followed by oil/water separation. The solvent was removed by evaporation. The residue was recrystallized successively from 15 ml of a 1:1:1 mixed solvent of chloroform, acetone, and ethanol and 150 ml of a 1:2 mixed solvent of dimethylformamide and ethanol to give a corresponding ClO4 or PF6 salt of compound No. 1 or a corresponding ClO4 salt of compound Nos. 2 to 6.

Provenance & Evidence