奈帕芬胺杂质1

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: A solution of 2-aminobenzophenone (100 g, 0.51 mol), urea (55 g, 0.93 mol) and acetic acid (300 mL) was stirred at 110° C. for 18 h. The reaction mixture was cooled to rt and filtered. The solid was washed with water and dried under reduced pressure. 4-Phenylquinazolin-2(1H)-one was isolated as a yellow solid and was used without further purification. filtered The solid was washed with water dried under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To a mixture of 15.0 parts of 2-aminobenzophenone, 45 volume parts of acetic acid and 2 volume parts of concentrated hydrochloric acid, a solution of 5.6 parts of sodium nitrite in 16 volume parts of water is added dropwise under ice-cooling and stirring. The mixture is then added dropwise to a solution of 15.0 parts of ethyl β-chloroacetoacetate and 20 parts of potassium acetate in a mixture of 160 volume parts of ethanol and 35 volume parts of water. After 15 minutes precipitated crystals are collected to yield ethyl (2-benzoylphenyl)azochloroacetate as crystals. Recrystallization from ethanol gives yellow needles melting at 119°-120°C. cooling After 15 minutes precipitated crystals are collected

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

实验步骤: To a mixture of 15.0 parts of 2-aminobenzophenone, 45 volume parts of acetic acid and 2 volume parts of concentrated hydrochloric acid, a solution of 5.6 parts of sodium nitrite in 16 volume parts of water is added dropwise under ice-cooling and stirring. The mixture is then added dropwise to a solution of 15.0 parts of ethyl β-chloroacetoacetate and 20 parts of potassium acetate in a mixture of 160 volume parts of ethanol and 35 volume parts of water. After 15 minutes precipitated crystals are collected to yield ethyl (2-benzoylphenyl)azochloroacetate as crystals. Recrystallization from ethanol gives yellow needles melting at 119°-120°C. cooling After 15 minutes precipitated crystals are collected

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

实验步骤: In the manner given in Preparation 1, 2-aminobenzophenone is refluxed with hydrazine hydrate in diethylene glycol to give 2-aminobenzophenone hydrazone.

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

实验步骤: In the manner given in Preparation 1, 2-aminobenzophenone is refluxed with hydrazine hydrate in diethylene glycol to give 2-aminobenzophenone hydrazone.