N-(2,3-dimethylphenyl)-3-oxobutanamide

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 10.3 g (50 m mol) of N-(2,3-dimethylphenyl)-3-oxo-butanamide, 4.50 g (75 m mol) of N,N-dimethylhydrazine and 60 ml of toluene was stirred for 8 hours at 60° C. Then, unreacted N,N-dimethylhydrazine and the resulting water together with about 10 ml of toluene were distilled off outside the reaction system. 10.5 g (125 m mol) of diketene was added dropwise to the remaining solution over a period of 5 minutes, while refluxing. The mixture was further refluxed for 2 hours and cooled to room temperature. The resulting crystals were filtered, washed and dried to obtain 8.63 g (yield 64%) of the title compound. Then, unreacted N,N-dimethylhydrazine and the resulting water together with about 10 ml of toluene were distilled off outside the reaction system 10.5 g (125 m mol) of diketene was added dropwise to the remaining solution over a period of 5 minutes while refluxing The mixture was further refluxed for 2 hours cooled to room temperature The resulting crystals were filtered washed dried

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 10.3 g (50 m mol) of N-(2,3-dimethylphenyl)-3-oxo-butanamide, 4.50 g (75 m mol) of N,N-dimethylhydrazine and 60 ml of toluene was stirred for 8 hours at 60° C. Then, unreacted N,N-dimethylhydrazine and the resulting water together with about 10 ml of toluene were distilled off outside the reaction system. 10.5 g (125 m mol) of diketene was added dropwise to the remaining solution over a period of 5 minutes, while refluxing. The mixture was further refluxed for 2 hours and cooled to room temperature. The resulting crystals were filtered, washed and dried to obtain 8.63 g (yield 64%) of the title compound. Then, unreacted N,N-dimethylhydrazine and the resulting water together with about 10 ml of toluene were distilled off outside the reaction system 10.5 g (125 m mol) of diketene was added dropwise to the remaining solution over a period of 5 minutes while refluxing The mixture was further refluxed for 2 hours cooled to room temperature The resulting crystals were filtered washed dried