反应详情

温度

60 °C

A solution of ethyl (S)-2-ethoxy-4-[N-{1-(2-piperidinophenyl)-3-methyl-1-butyl}-aminocarbonylmethyl]benzoate (20 g, 41.6 mmol) in denatured spirit (200 ml) was stirred at 60–65° C. and 1N sodium hydroxide solution (62 ml) was added. After two hours of stirring at 60° C., the reaction mixture was cooled to 35° C. and pH was adjusted to about 5.0 using 1N hydrochloric acid (about 70 ml). The solution was stirred for 30 minutes at 35–40° C., cooled to 0° C. and stirred at 0 to 5° C. for one hour to get a crystalline product. The crystals were separated by filtration and washed with water. The product was dried at 60–65° C. under vacuum to get repaglinide (17.8 g, Yield: 94%, Assay 99.5% by HPLC).

1. temperaturethe reaction mixture was cooled to 35° C.
2. stirringThe solution was stirred for 30 minutes at 35–40° C.
3. temperaturecooled to 0° C.
4. stirringstirred at 0 to 5° C. for one hour
5. customto get a crystalline product
6. customThe crystals were separated by filtration
7. washwashed with water
8. customThe product was dried at 60–65° C. under vacuum