反应详情

In a 50 ml three-necked flask, place 1.615 g of 7-nitro-9-oxo-9H-fluorene-4-carboxylic acid, which can be obtained according to WO2003057145, in suspension in 30 ml of dichloromethane, and then add successively 567 μl of oxalyl chloride and 1 drop of dimethylformamide. After stirring for 4 hours at room temperature, add 0.779 g of 1,2-diaminobenzene and 1.686 ml of triethylamine. After stirring for 20 hours at room temperature, the precipitate that formed is filtered off, and washed with water, then with a 10% saturated aqueous solution of sodium hydrogen carbonate and, finally, with water. After formation of a paste with diisopropyl ether, in this way we obtain 1.6 g of (2-aminophenyl)amide of 7-nitro-9-oxo-9H-fluoren -4-carboxylic acid, in the form of an orange powder, which is used as it is in the following stage, with the following characteristics:

1. stirringAfter stirring for 20 hours at room temperature
2. customthe precipitate that formed
3. filtrationis filtered off
4. washwashed with water