HCID 12900263, compound → HCID 131712311, compound

Participants

Reaction Steps

To a stirred solution of 13.6 g. of 5-amino-1,2,3-benzenetricarboxylic acid, triphenyl ester (U.S. Pat. No. 4,087,613) in 45 ml. of dry pyridine is added 4.58 g. of 8-chloro-1,3,5-naphthalenetrisulfonyl chloride, and the mixture is heated at 60°-70° C. for three hours. The cooled solution is added slowly with vigorous stirring to 300 ml. of ice-water, and the resulting solid is collected by filtration, washed with water, and dried. The solid is dissolved in methylene chloride, washed with water, and dried. The extract is concentrated to a volume of 80 ml. and passed through a bed of hydrous magnesium silicate. Evaporation of the filtrate with the addition of ether gives a solid, which is purified by chromatography on silica gel giving 7.8 g. of a light yellow solid.

Provenance & Evidence