反应详情

To a solution chloroacetyl chloride (1.2 mL, 15.2 mmol) in DCM (65 mL) at 0° C. was added dropwise a solution of 2,2′-(iminodi-2,1-ethanediyl)bis(1H-isoindole-1,3(2H)-dione) (5 g, 13.7 mmol) [prepared according to Anelli, P. L.; et. al. J. Org. Chem. 1984 49, 4197.] and Et3N (2.5 mL, 17.9 mmol) in DCM (65 mL). After 1 h, the solution was partitioned between H2O-DCM and the aqueous phase was washed several times with DCM. The combined organic fractions were dried (Na2SO4), concentrated and purified via column chromatography (silica, 5% MeOH in DCM (NH4OH)) yielding the title compound (5.9 g, 98%) as a yellow foam: LCMS (ES) m/e 440 (M+H)+.

1. customthe solution was partitioned between H2O-DCM
2. washthe aqueous phase was washed several times with DCM
3. dry with materialThe combined organic fractions were dried (Na2SO4)
4. concentrationconcentrated
5. custompurified via column chromatography (silica, 5% MeOH in DCM (NH4OH))