乙基 2-(N-甲酰氨基)乙酸甲酯

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

实验步骤: Phenylglycine ethyl ester hydrochloride (21.5 g; 0.1 mol) was dissolved in 200 ml of formic acid, whereto sodium formate (8.16 g; 1.2 eq.) was added, followed by adding dropwise acetic anhydride (20 ml; 2.1 eq.). After two hours' stirring, 10 ml of acetic anhydride was added dropwise, and the mixture was stirred at 50°-60° C. for 1.5 hours. After the solvent was distilled off, the residue was neutralized with an aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solvent was distilled off to afford an oily product. the mixture was stirred at 50°-60° C. for 1.5 hours After the solvent was distilled off extracted with ethyl acetate The organic layer was washed with a saturated aqueous solution of sodium chloride dried over magnesium sulfate The solvent was distilled off to afford an oily product

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: Phenylglycine ethyl ester hydrochloride (21.5 g; 0.1 mol) was dissolved in 200 ml of formic acid, whereto sodium formate (8.16 g; 1.2 eq.) was added, followed by adding dropwise acetic anhydride (20 ml; 2.1 eq.). After two hours' stirring, 10 ml of acetic anhydride was added dropwise, and the mixture was stirred at 50°-60° C. for 1.5 hours. After the solvent was distilled off, the residue was neutralized with an aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solvent was distilled off to afford an oily product. the mixture was stirred at 50°-60° C. for 1.5 hours After the solvent was distilled off extracted with ethyl acetate The organic layer was washed with a saturated aqueous solution of sodium chloride dried over magnesium sulfate The solvent was distilled off to afford an oily product

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: Phenylglycine ethyl ester hydrochloride (21.5 g; 0.1 mol) was dissolved in 200 ml of formic acid, whereto sodium formate (8.16 g; 1.2 eq.) was added, followed by adding dropwise acetic anhydride (20 ml; 2.1 eq.). After two hours' stirring, 10 ml of acetic anhydride was added dropwise, and the mixture was stirred at 50°-60° C. for 1.5 hours. After the solvent was distilled off, the residue was neutralized with an aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solvent was distilled off to afford an oily product. the mixture was stirred at 50°-60° C. for 1.5 hours After the solvent was distilled off extracted with ethyl acetate The organic layer was washed with a saturated aqueous solution of sodium chloride dried over magnesium sulfate The solvent was distilled off to afford an oily product

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

实验步骤: Absolute ethanol (50 mL) was slowly added to a mechanically stirred suspension of finely cut sodium metal (19.3 g; 0.84 mol) in anhydrous ether (500 mL). When most of the metal had dissolved, diethyl oxalate (114 mL; 0.84 mol) was slowly added followed by the slow addition of the N-phenyl-N-formylglycine ethyl ester (130 g; 0.67 mol). The mixture was stirred at room temperature overnight and then ice-water (700 mL) was added. The resulting emulsion was broken by sequential addition of a saturated sodium chloride solution (150 mL) and water (200 mL). The aqueous layer was removed, potassium thiocyanate (114 g; 1.18 mol) was added, then concentrated hydrochloric acid (160 mL), followed by absolute ethanol (900 mL). The resultant mixture was warmed at 60°-65° C. for 1 hour, then at 50° C. for 6 hours and finally allowed to stir at room temperature overnight. The light yellow precipitate was filtered, washed with ethanol and dried to give 103 g (48%) of diethyl 2-mercapto-1-phenyl-4,5-imidazoledicarboxylate (mp 145°-146° C.). When most of the metal had dissolved The aqueous layer was removed at 50° C. for 6 hours to stir at room temperature overnight The light yellow precipitate was filtered washed with ethanol dried

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

实验步骤: N-Phenylglycine ethyl ester (100 g; 0-56 mol) was added in small portions to acetic formic anhydride (100 g; 1.14 mol) with vigorous stirring. The mixture was allowed to stir overnight, then it was poured into water, and extracted with ether. The ether solution was washed with sodium bicarbonate solution and then with water. The ether was evaporated in vacuo to give an oil which was distilled to give N-phenyl-N-formylglycine ethyl ester (81 g; 70%) having a bp 115°-117° C. extracted with ether The ether solution was washed with sodium bicarbonate solution The ether was evaporated in vacuo to give an oil which was distilled