1-(4-溴-3-氟苯基)咪唑烷-2,4-二酮

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

实验步骤: To a solution of ethyl 2-(4-bromo-3-fluoro-anilino)acetate (86 g, 0.31 mol) in acetic acid (1.5 L) and water (100 mL) was added a solution of potassium cyanate (50 g, 0.6 mol) in water (200 mL). The reaction mixture was stirred at room temperature for 12 h and then evaporated to dryness. Then 1.5 L of 25% HCl was added to the residue and the mixture was heated to reflux for 3 h. After cooling to room temperature, the solid was filtered and dried to give the title compound. LC-MS: calculated for C9H6BrFN2O2 271.96 observed m/e: 273.35 (M+H)+ (Rt 3.44/6.5 min). evaporated to dryness Then 1.5 L of 25% HCl was added to the residue the mixture was heated to reflux for 3 h After cooling to room temperature the solid was filtered dried

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

实验步骤: To a solution of ethyl 2-(4-bromo-3-fluoro-anilino)acetate (86 g, 0.31 mol) in acetic acid (1.5 L) and water (100 mL) was added a solution of potassium cyanate (50 g, 0.6 mol) in water (200 mL). The reaction mixture was stirred at room temperature for 12 h and then evaporated to dryness. Then 1.5 L of 25% HCl was added to the residue and the mixture was heated to reflux for 3 h. After cooling to room temperature, the solid was filtered and dried to give the title compound. LC-MS: calculated for C9H6BrFN2O2 271.96 observed m/e: 273.35 (M+H)+ (Rt 3.44/6.5 min). evaporated to dryness Then 1.5 L of 25% HCl was added to the residue the mixture was heated to reflux for 3 h After cooling to room temperature the solid was filtered dried

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

实验步骤: To a solution of ethyl 2-(4-bromo-3-fluoro-anilino)acetate (86 g, 0.31 mol) in acetic acid (1.5 L) and water (100 mL) was added a solution of potassium cyanate (50 g, 0.6 mol) in water (200 mL). The reaction mixture was stirred at room temperature for 12 h and then evaporated to dryness. Then 1.5 L of 25% HCl was added to the residue and the mixture was heated to reflux for 3 h. After cooling to room temperature, the solid was filtered and dried to give the title compound. LC-MS: calculated for C9H6BrFN2O2 271.96 observed m/e: 273.35 (M+H)+ (Rt 3.44/6.5 min). evaporated to dryness Then 1.5 L of 25% HCl was added to the residue the mixture was heated to reflux for 3 h After cooling to room temperature the solid was filtered dried