6-氟-2,3-二氢-1H-喹啉-4-酮

反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 33.0 parts of 6-fluoro-4-oxo-1,2,3,4-tetrahydroquinoline and 200 parts of dioxane were mixed, and 39.6 parts of phosgene were introduced to the stirred mixture over about 30 minutes while the temperature was maintained at 20°-25° C. After the introduction, the temperature was raised gradually, and the reaction was effected at 40°-45° C. for 2.5 hours, after which the temperature was further raised to 70° C., nitrogen gas was passed through the mixture, and the solvent (dioxane) was distilled off under reduced pressure. Petroleum ether was added to the residue followed by filtration, washing and drying, and there was obtained 43.7 parts of 6-fluoro-4-oxo-1-chloroformyl-1,2,3,4-tetrahydroquinoline. was maintained at 20°-25° C After the introduction, the temperature was raised gradually the solvent (dioxane) was distilled off under reduced pressure Petroleum ether was added to the residue followed by filtration washing drying

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 500 mg of 1-(4-fluorophenyl)azetidin-2-one (Example 154A, 3.03 mmol, 1 equivalent) were initially charged in 24 ml of dichloromethane, 0.5 ml of trifluoromethanesulphonic acid (909 mg, 6.05 mmol, 2 equivalents) were added at 0° C. and the mixture was stirred at RT for 45 min. Two more times, 0.3 equivalents of trifluoromethanesulphonic acid were added, and after each addition the mixture was stirred for 30 min. With ice cooling, saturated aqueous sodium bicarbonate solution was added carefully, and the reaction mixture was extracted three times with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated. This gave 284 mg (57% of theory) of the title compound. after each addition the mixture was stirred for 30 min the reaction mixture was extracted three times with dichloromethane The combined organic phases were dried over sodium sulphate filtered concentrated

反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 33.0 parts of 6-fluoro-4-oxo-1,2,3,4-tetrahydroquinoline and 200 parts of dioxane were mixed, and 39.6 parts of phosgene were introduced to the stirred mixture over about 30 minutes while the temperature was maintained at 20°-25° C. After the introduction, the temperature was raised gradually, and the reaction was effected at 40°-45° C. for 2.5 hours, after which the temperature was further raised to 70° C., nitrogen gas was passed through the mixture, and the solvent (dioxane) was distilled off under reduced pressure. Petroleum ether was added to the residue followed by filtration, washing and drying, and there was obtained 43.7 parts of 6-fluoro-4-oxo-1-chloroformyl-1,2,3,4-tetrahydroquinoline. was maintained at 20°-25° C After the introduction, the temperature was raised gradually the solvent (dioxane) was distilled off under reduced pressure Petroleum ether was added to the residue followed by filtration washing drying