N,N'-双(2-甲基丙基)乙烷-1,2-二胺

反应条件: temp:7.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 7-amino-3-(1-sulfomethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (5 g) was dissolved in water (19 ml) using 30% w/w sodium hydroxide (1.5 g in 8 ml water) and sodium bicarbonate (1 g), O-formylmandeloyl chloride (2.45 g) was added at 0-5° C. and maintained at 5-10° C. over a period of 1-2 hours. After the completion of reaction, the reaction mixture was acidified with conc. HCl (2.6 g) and maintained the reaction at 28-30° C. for about 2-3 hrs, sodium bicarbonate (3.5 g) was added to set the pH 5±1 and the reaction mass solution was added to a solution of N,N′-diisobutylethylenediamine diacetate (8.2 g) in water (40 mL) and isopropyl alcohol (40 mL) and stirred well at 25-30° C. for about 2-3 hours. The reaction mixture was cooled to 5-10° C., filtered, washed with chilled water (0-5° C.) followed by isopropyl alcohol (0-5° C.) and dried the material at ˜40° C. to get N,N′-diisobutylethylenediamine salt of 7-D-mandelamido-3-(((1-sulfomethyl-1H-tetrazol-5-yl)thio)methyl)-3-cephem-4-carboxylic acid (5.5 g). Step(ii) was added at 0-5° C. After the completion of reaction maintained the reaction at 28-30° C. for about 2-3 hrs The reaction mixture was cooled to 5-10° C. filtered washed with chilled water (0-5° C.) followed by isopropyl alcohol (0-5° C.) dried the material at ˜40° C.

反应条件: temp:7.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 7-amino-3-(1-sulfomethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (5 g) was dissolved in water (19 ml) using 30% w/w sodium hydroxide (1.5 g in 8 ml water) and sodium bicarbonate (1 g), O-formylmandeloyl chloride (2.45 g) was added at 0-5° C. and maintained at 5-10° C. over a period of 1-2 hours. After the completion of reaction, the reaction mixture was acidified with conc. HCl (2.6 g) and maintained the reaction at 28-30° C. for about 2-3 hrs, sodium bicarbonate (3.5 g) was added to set the pH 5±1 and the reaction mass solution was added to a solution of N,N′-diisobutylethylenediamine diacetate (8.2 g) in water (40 mL) and isopropyl alcohol (40 mL) and stirred well at 25-30° C. for about 2-3 hours. The reaction mixture was cooled to 5-10° C., filtered, washed with chilled water (0-5° C.) followed by isopropyl alcohol (0-5° C.) and dried the material at ˜40° C. to get N,N′-diisobutylethylenediamine salt of 7-D-mandelamido-3-(((1-sulfomethyl-1H-tetrazol-5-yl)thio)methyl)-3-cephem-4-carboxylic acid (5.5 g). Step(ii) was added at 0-5° C. After the completion of reaction maintained the reaction at 28-30° C. for about 2-3 hrs The reaction mixture was cooled to 5-10° C. filtered washed with chilled water (0-5° C.) followed by isopropyl alcohol (0-5° C.) dried the material at ˜40° C.

反应条件: temp:7.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 7-amino-3-(1-sulfomethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (5 g) was dissolved in water (19 ml) using 30% w/w sodium hydroxide (1.5 g in 8 ml water) and sodium bicarbonate (1 g), O-formylmandeloyl chloride (2.45 g) was added at 0-5° C. and maintained at 5-10° C. over a period of 1-2 hours. After the completion of reaction, the reaction mixture was acidified with conc. HCl (2.6 g) and maintained the reaction at 28-30° C. for about 2-3 hrs, sodium bicarbonate (3.5 g) was added to set the pH 5±1 and the reaction mass solution was added to a solution of N,N′-diisobutylethylenediamine diacetate (8.2 g) in water (40 mL) and isopropyl alcohol (40 mL) and stirred well at 25-30° C. for about 2-3 hours. The reaction mixture was cooled to 5-10° C., filtered, washed with chilled water (0-5° C.) followed by isopropyl alcohol (0-5° C.) and dried the material at ˜40° C. to get N,N′-diisobutylethylenediamine salt of 7-D-mandelamido-3-(((1-sulfomethyl-1H-tetrazol-5-yl)thio)methyl)-3-cephem-4-carboxylic acid (5.5 g). Step(ii) was added at 0-5° C. After the completion of reaction maintained the reaction at 28-30° C. for about 2-3 hrs The reaction mixture was cooled to 5-10° C. filtered washed with chilled water (0-5° C.) followed by isopropyl alcohol (0-5° C.) dried the material at ˜40° C.