Carbon Dioxide → HCID 69225377, compound

Participants

Reaction Conditions

Reaction Steps

In a 50 ml flask, 1.17 g (6.5 mmol) of isophtalic acid monomethyl ester are dissolved in 10 ml of DMF. To this solution, 1.16 g (7.2 mmol, 1.1 eq.) of 1,1′-carbonyl-diimidazole is added at room temperature under nitrogen. The mixture is stirred until carbon dioxide formation stops. Then, 1.00 g (6.5 mmol) of 4-fluoro-N-hydroxy-benzamidine is added and the resulting yellow solution stirred for 2 h. Now, another 1.16 g (7.2 mmol, 1.1 eq.) of 1,1′-carbonyl-diimidazole are added and the mixture is heated to 115° C. After 2 h at this temperature, the reaction mixture is cooled to room temperature and the solvent removed in vacuo. After chromatographical purification (160 g SiO2;eluent: hexane/CH2Cl2 6:4 to 1:1) the title compound is obtained as a white solid. Mass spectrum: m/z (M+H)+: 299.0

Provenance & Evidence