乙基 3-(2-氟苯胺基)-3-氧代丙酸乙酯

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of the product from step 1 (20.27 g) in DCM (100 ml) was added to polyphosphoric acid (43.7 ml). Dichloromethane was distilled from the reaction mixture by increasing the temperature slowly and then the brownish gummy solution was stirred at 120° C. for 3 hours and then left at room temperature for 16 hours. The reaction mixture was quenched by adding ice cooled water and the product was filtered. The filter cake was stirred with 500 mL of water and filtered to give the desired product (9.38 g) as a colorless solid. LRMS (ES+) m/z 180.1 (M+H)+. Dichloromethane was distilled from the reaction mixture by increasing the temperature slowly left at room temperature for 16 hours The reaction mixture was quenched by adding ice cooled water the product was filtered The filter cake was stirred with 500 mL of water filtered

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of the product from step 1 (20.27 g) in DCM (100 ml) was added to polyphosphoric acid (43.7 ml). Dichloromethane was distilled from the reaction mixture by increasing the temperature slowly and then the brownish gummy solution was stirred at 120° C. for 3 hours and then left at room temperature for 16 hours. The reaction mixture was quenched by adding ice cooled water and the product was filtered. The filter cake was stirred with 500 mL of water and filtered to give the desired product (9.38 g) as a colorless solid. LRMS (ES+) m/z 180.1 (M+H)+. Dichloromethane was distilled from the reaction mixture by increasing the temperature slowly left at room temperature for 16 hours The reaction mixture was quenched by adding ice cooled water the product was filtered The filter cake was stirred with 500 mL of water filtered

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

实验步骤: To a solution of 2-fluoroaniline (8.67 ml) in ethyl acetate (266 ml) was added water (200 ml) and sodium bicarbonate (15.12 g). Ethyl malonyl chloride (13.82 ml) was added and the solution was stirred at room temperature for 1 hour. The two layers were separated and the organic phase was washed with a saturated aqueous solution of sodium bicarbonate, water and brine, dried over sodium sulfate and evaporated to provide a brownish oil. The crude reaction mixture was used directly in the next step. LRMS (ES+) m/z 226.1 (M+H)+. The two layers were separated the organic phase was washed with a saturated aqueous solution of sodium bicarbonate, water and brine dried over sodium sulfate evaporated to provide a brownish oil The crude reaction mixture

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

实验步骤: To a solution of 2-fluoroaniline (8.67 ml) in ethyl acetate (266 ml) was added water (200 ml) and sodium bicarbonate (15.12 g). Ethyl malonyl chloride (13.82 ml) was added and the solution was stirred at room temperature for 1 hour. The two layers were separated and the organic phase was washed with a saturated aqueous solution of sodium bicarbonate, water and brine, dried over sodium sulfate and evaporated to provide a brownish oil. The crude reaction mixture was used directly in the next step. LRMS (ES+) m/z 226.1 (M+H)+. The two layers were separated the organic phase was washed with a saturated aqueous solution of sodium bicarbonate, water and brine dried over sodium sulfate evaporated to provide a brownish oil The crude reaction mixture

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of the product from step 1 (20.27 g) in DCM (100 ml) was added to polyphosphoric acid (43.7 ml). Dichloromethane was distilled from the reaction mixture by increasing the temperature slowly and then the brownish gummy solution was stirred at 120° C. for 3 hours and then left at room temperature for 16 hours. The reaction mixture was quenched by adding ice cooled water and the product was filtered. The filter cake was stirred with 500 mL of water and filtered to give the desired product (9.38 g) as a colorless solid. LRMS (ES+) m/z 180.1 (M+H)+. Dichloromethane was distilled from the reaction mixture by increasing the temperature slowly left at room temperature for 16 hours The reaction mixture was quenched by adding ice cooled water the product was filtered The filter cake was stirred with 500 mL of water filtered

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

实验步骤: To a solution of 2-fluoroaniline (8.67 ml) in ethyl acetate (266 ml) was added water (200 ml) and sodium bicarbonate (15.12 g). Ethyl malonyl chloride (13.82 ml) was added and the solution was stirred at room temperature for 1 hour. The two layers were separated and the organic phase was washed with a saturated aqueous solution of sodium bicarbonate, water and brine, dried over sodium sulfate and evaporated to provide a brownish oil. The crude reaction mixture was used directly in the next step. LRMS (ES+) m/z 226.1 (M+H)+. The two layers were separated the organic phase was washed with a saturated aqueous solution of sodium bicarbonate, water and brine dried over sodium sulfate evaporated to provide a brownish oil The crude reaction mixture