Ac-DL-脯氨酸-OH

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:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 11.8 g (75 m mol) of N-Acetyl-DL-proline and 10.5 ml (75 m mol) of triethylamine in 150 ml dichloromethane at -15° C., is added 9.75 ml (75 m mol) of isobutyl chloroformate. The reaction mixture is stirred at about -10° C. for 30 min. To this reaction mixture is added a cold solution of 11.5 g (50 m mol) of 6-(4-aminophenyl)-1,2-dihydro-2-oxonicotinic acid and 7.7 ml (55 m mol) triethylamine in 200 ml of N,N-dimethylacetamide, which is stirred while cooling in an ice bath for 3 hrs, then overnight at room temperature. The reaction mixture is evaporated to dryness, the residue is triturated with water, and the solid collected by filtration. The solid is washed with water and acetonitrile and dried to yield 13.2 g of 6-[4-(N-Acetyl-DL-prolylamino)phenyl]-1,2-dihydro-2-oxonicotinic acid, m.p. 279°-281° dec. is stirred while cooling in an ice bath for 3 hrs overnight at room temperature The reaction mixture is evaporated to dryness the residue is triturated with water the solid collected by filtration The solid is washed with water and acetonitrile dried

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 11.8 g (75 m mol) of N-Acetyl-DL-proline and 10.5 ml (75 m mol) of triethylamine in 150 ml dichloromethane at -15° C., is added 9.75 ml (75 m mol) of isobutyl chloroformate. The reaction mixture is stirred at about -10° C. for 30 min. To this reaction mixture is added a cold solution of 11.5 g (50 m mol) of 6-(4-aminophenyl)-1,2-dihydro-2-oxonicotinic acid and 7.7 ml (55 m mol) triethylamine in 200 ml of N,N-dimethylacetamide, which is stirred while cooling in an ice bath for 3 hrs, then overnight at room temperature. The reaction mixture is evaporated to dryness, the residue is triturated with water, and the solid collected by filtration. The solid is washed with water and acetonitrile and dried to yield 13.2 g of 6-[4-(N-Acetyl-DL-prolylamino)phenyl]-1,2-dihydro-2-oxonicotinic acid, m.p. 279°-281° dec. is stirred while cooling in an ice bath for 3 hrs overnight at room temperature The reaction mixture is evaporated to dryness the residue is triturated with water the solid collected by filtration The solid is washed with water and acetonitrile dried