反应详情

A mixture of 4-(2-chloroethyl)morpholine hydrochloride (0.195 g, 1.050 mmol), K2CO3 (0.242 g, 1.751 mmol) and tert-butyl 2-(5-(methylsulfonamidomethyl)-1,3-dioxoisoindolin-2-yl)acetate (0.258 g, 0.700 mmol), (prepared in an analogous manner as described in Example 46, Scheme 46, Steps 1, 2, 3, 4), was heated to 80° C. for 5 hours in DMF (10 ml) and then stirred at room temperature overnight. The insoluble inorganic salts were filtered off and then washed with ethyl acetate. The filtrate was concentrated to dryness, and the resulting crude was purified by filtration through a silica gel cartridge (100% DCM to DCM:MeOH=98:2) to afford tert-butyl 2-(5-((N-(2-morpholinoethyl)methylsulfonamido)methyl)-1,3-dioxoisoindolin-2-yl)acetate (0.200 g, 0.415 mmol, 59.3% yield, MS/ESI+ 482.1 [MH]+).

1. custom(prepared in an analogous manner
2. filtrationThe insoluble inorganic salts were filtered off
3. washwashed with ethyl acetate
4. concentrationThe filtrate was concentrated to dryness
5. filtrationthe resulting crude was purified by filtration through a silica gel cartridge (100% DCM to DCM:MeOH=98:2)