反应详情

A cooled (0° C.) solution of 5-chloro-2,4-dimethoxyaniline (5 g) in DCM under an atmosphere of argon is treated dropwise with bromoacetyl bromide (2.4 ml). After 5 minutes, TEA (7.5 ml) is added dropwise and after stirring for 20 minutes the reaction mixture is diluted with water and extracted with DCM). The organic phase is washed with distilled water, dried over Na2SO4, filtered and evaporated to give a beige solid. This is purified by flash column chromatography on silica, eluting with 20-100% n-hexane in DCM to afford the title compound. [M+H]+ 308.

1. extractionextracted with DCM)
2. washThe organic phase is washed with distilled water
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customto give a beige solid
7. customThis is purified by flash column chromatography on silica
8. washeluting with 20-100% n-hexane in DCM