preparation | 2-methyl -3-nitrobenzoic acid (5g) is dissolved in methanol (50ml), concentrated sulfuric acid (5ml) is added, heated and refluxed overnight, the next day, the reaction is stopped, methanol is evaporated, EA is dissolved, EA layer is successively washed with saturated sodium bicarbonate solution, saturated salt water is washed, anhydrous sodium sulfate is dried, and 4g compound S-103-1 is concentrated. The compound S-103-1(3.5g) is dissolved in CCl4, NBS(3.5g) and AIBN(600mg) are added, heated and refluxed overnight, the reaction is stopped the next day, cooled to room temperature, filtered, diluted with CH2Cl2, washed with saturated salt water, dried with anhydrous sodium sulfate, and concentrated to obtain compound S-103-2. The S-103-2 of the compound is dissolved in methanol solution, ammonia methanol solution is added, heated and refluxed, the reaction is complete for 2 hours, the product is filtered, the filtrate is concentrated, column chromatography is carried out, and 3.6g compound compound S-103-3 is combined. Compound compound S-103-3(1.5g) is dissolved in methanol, Pd/C(200mg) is added, H2 is introduced, the reaction is complete, filtration is carried out, and 1g compound compound S-103, namely 4-amino-isoindolin-1-one, is concentrated. |