2-amino-N-methyl-N-phenylacetamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 5.0 g (0.026 moles) N-methyl 2-nitro acetanilide in 250 mL absolute alcohol is added 0.5 g of 10% palladium on activated carbon. The nitro functional group is reduced to amino functionality under catalytic reduction with hydrogen gas in a pressure bottle at 60 PSI using Parr hydrogenation apparatus. The reduction is carried out for five hours by which time the reaction is complete as indicated by no further consumption of H2 gas. The reaction mixture is filtered and the solvent from the filtrate is removed under reduced pressure. To the crude residue a small amount of mixture of ethyl acetate ethanol is added and cooled. The resulting precipitate is filtered and washed with cold ethyl acetate in ethanol solvent and dried to give the desired compound N-methyl 2-amino acetanilide. as indicated by no further consumption of H2 gas The reaction mixture is filtered the solvent from the filtrate is removed under reduced pressure To the crude residue a small amount of mixture of ethyl acetate ethanol is added cooled The resulting precipitate is filtered washed with cold ethyl acetate in ethanol solvent dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 5.0 g (0.026 moles) N-methyl 2-nitro acetanilide in 250 mL absolute alcohol is added 0.5 g of 10% palladium on activated carbon. The nitro functional group is reduced to amino functionality under catalytic reduction with hydrogen gas in a pressure bottle at 60 PSI using Parr hydrogenation apparatus. The reduction is carried out for five hours by which time the reaction is complete as indicated by no further consumption of H2 gas. The reaction mixture is filtered and the solvent from the filtrate is removed under reduced pressure. To the crude residue a small amount of mixture of ethyl acetate ethanol is added and cooled. The resulting precipitate is filtered and washed with cold ethyl acetate in ethanol solvent and dried to give the desired compound N-methyl 2-amino acetanilide. as indicated by no further consumption of H2 gas The reaction mixture is filtered the solvent from the filtrate is removed under reduced pressure To the crude residue a small amount of mixture of ethyl acetate ethanol is added cooled The resulting precipitate is filtered washed with cold ethyl acetate in ethanol solvent dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The same procedures as Example 1 are repeated except that 4-chloro-6-methyl-2-phenylpyrimidine and 2-amino-N-methyl-N-phenylacetamide are used instead of 4-chloro-5,6-dimethyl-2-phenylpyrimidine and 2-amino-N,N-dipropylacetamide, respectively. The product thus obtained is recrystallized from isopropanol to give the desired compound, m.p. 134-136° C. The product thus obtained is recrystallized from isopropanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 5.0 g (0.026 moles) N-methyl 2-nitro acetanilide in 250 mL absolute alcohol is added 0.5 g of 10% palladium on activated carbon. The nitro functional group is reduced to amino functionality under catalytic reduction with hydrogen gas in a pressure bottle at 60 PSI using Parr hydrogenation apparatus. The reduction is carried out for five hours by which time the reaction is complete as indicated by no further consumption of H2 gas. The reaction mixture is filtered and the solvent from the filtrate is removed under reduced pressure. To the crude residue a small amount of mixture of ethyl acetate ethanol is added and cooled. The resulting precipitate is filtered and washed with cold ethyl acetate in ethanol solvent and dried to give the desired compound N-methyl 2-amino acetanilide. as indicated by no further consumption of H2 gas The reaction mixture is filtered the solvent from the filtrate is removed under reduced pressure To the crude residue a small amount of mixture of ethyl acetate ethanol is added cooled The resulting precipitate is filtered washed with cold ethyl acetate in ethanol solvent dried