反应详情

温度

27.5 °C

In a four neck round bottom flask, charged methanol (100 ml), 2-([(5S)-2-Oxo-3-[4-(3-oxo-4-morpholinyl)phenyl]-1,3-oxazolidin-5-yl}methyl)-1H-isoindole-1,3(2H)-dione (10 g), and 40% aqueous methylamine (5 g) at 25 to 30° C. Reaction mass is stirred for 1 h at 25 to 30° C. Added second lot of 40% aqueous methylamine (5 g) to reaction mass at 25 to 30° C. After complete addition of methylamine solution, reaction mass is heated to 60 to 65° C., and maintained at same temperature for 4 h. Reaction mixture then cooled to 25 to 30° C. and added conc. hydrochloric acid (2 ml, pH should be 1 to 2). Finally reaction mass is cooled to 10° C. and stirred for 30 minutes. Obtained solid is filtered off and washed by chilled methanol (10 ml). Yield 80%

1. customReaction mass
2. customto reaction mass at 25 to 30° C
3. temperatureis heated to 60 to 65° C.
4. temperaturemaintained at same temperature for 4 h
5. customReaction mixture
6. temperaturethen cooled to 25 to 30° C.
7. customFinally reaction mass
8. temperatureis cooled to 10° C.
9. stirringstirred for 30 minutes
10. customObtained solid
11. filtrationis filtered off
12. washwashed
13. temperatureby chilled methanol (10 ml)