反应详情

A mixture of 3.93 g (30 mmol) of N-acetyl-L-alanine, 3.3 ml (30 mmol) of N-methyl morpholine, 2.33 ml (30 mmol) of methyl chloroformate, and 80 ml of acetonitrile is stirred at -10° to -20° for 30 minutes. A mixture of 4.08 g (20 mmol) of 8-amino-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, 8.4 ml (60 mmol) of triethylamine, 7.6 ml (60 mmol) of chlorotrimethylsilane, and 100 ml of dichloromethane was stirred at room temperature for 40 minutes and then cooled to -20°. The cold mixed anhydride is added to the cold silylated quinoline and stirred for 4 hours with cooling and overnight at room temperature. The reaction mixture is evaporated to dryness and the residue is treated with acetonitrile and 1N hydrochloric acid. The solid is filtered to give 3.03 g of 8-[[2-(acetylamino)-1-oxopropyl]amino]-1,4-dihydro-4 -oxo-3-quinolinecarboxylic acid.

1. stirringwas stirred at room temperature for 40 minutes
2. temperaturecooled to -20°
3. stirringstirred for 4 hours
4. customThe reaction mixture is evaporated to dryness
5. additionthe residue is treated with acetonitrile and 1N hydrochloric acid
6. filtrationThe solid is filtered