反应详情

1.0 g of 3-methylsulphonyl-4-(4-BOC-aminopiperidino)benzoic acid [obtainable by reacting methyl 3-methylsulphonyl-4-fluorobenzoate with 4-BOC-aminopiperidine and subsequently hydrolyzing the product to give the free acid] is dissolved in 15 ml of 1-methylpyrrolidone, and 0.67 g of 1-methyl-2-chloropyridinium chloride is added to this solution, which is stirred for 15 min. 0.9 g of guanidinium chloride and 2.6 ml of diisopropylethylamine are then added and the mixture is stirred at room temperature for 1 hr. After customary working-up, and after chromatography on silica gel (flash process, ethylacetate/10% methanol), N-diaminomethylene-3-methylsulphonyl-4-(4-BOC-aminopiperidino)benzamide is obtained.

1. customto give the free acid]
2. stirringthe mixture is stirred at room temperature for 1 hr