Phosphorus oxychloride → HCID 73676527, compound

Participants

Reaction Steps

Phosphoryl chloride (1.0 ml) is added to a stirred suspension of 1,3-Bis(1-methyl-2-(1H)-quinolylidene)acetone (0.68 g, 0.002 mol) in pyridine (10 ml). The mixture is stirred for 5 min., then the solid is collected and washed with a little pyridine, then with ether. The dye is converted to its perchlorate salt by solution in methanol, followed by addition of aqueous sodium perchlorate solution. After recrystallization from acetonitrile, the yield of purified dye is 0.30 g (36%) with the melting point indistinct. The following two dyes were prepared by procedures similar to that described above: 1,3-Diethyl-2[(1,3-diethyl-1H-imidazo[4,5 -b]quinoxalin-2-(3H)-ylidene)-1-propynyl]-1H-imidazo[4,5 -b]quinoxalinium perchlorate. ##STR19## Recrystallized from acetonitrile. Purified yield 35%. mp >300°. 1,3,3-Trimethyl-2-[(1,3,3-trimethyl-2-indolinylidene)-1-propynyl]-3H-indolium perchlorate. ##STR20## Recrystallized from methanol. Purified yield 43% mp 194-7° dec.

Provenance & Evidence