반응 #2275683

반응 방정식

2,4,6-Triiodo-5-methylamino-isophthaloyl dichloride

acetoxyacetyl chloride

→

acetic acid [(3,5-bis-chlorocarbonyl-2,4,6-triiodo-phenyl)-methyl-carbamoyl]-methyl ester

수율 69.8%

용매

ethyl acetate

DMA

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONThe reaction mixture was poured slowly onto ice-water (300 ml)
2. 2
   기타a white solid was isolated by filtration
3. 3
   세척washed with water
4. 4
   기타The ethyl acetate was collected
5. 5
   건조dried over MgSO4
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타to give a white solid
9. 9
   기타This was purified by silica column chromatography
10. 10
    세척eluting with petrol

실험 절차

2,4,6-Triiodo-5-methylamino-isophthaloyl dichloride (20 g, 32.8 mmol) was dissolved in DMA (60 ml) and acetoxyacetyl chloride (15.32 ml, 142 mmol) was added. The reaction was stirred overnight at room temperature with nitrogen bubbling through the reaction mixture. The reaction mixture was poured slowly onto ice-water (300 ml) and a white solid was isolated by filtration. The solid was dissolved in ethyl acetate and washed with water. The ethyl acetate was collected, dried over MgSO4, filtered and evaporated to give a white solid. This was purified by silica column chromatography eluting with petrol:ethyl acetate to give acetic acid [(3,5-bis-chlorocarbonyl-2,4,6-triiodo-phenyl)-methyl-carbamoyl]-methyl ester (16.25 g, 22.9 mmol).

출처