反应详情

TO a solution of 23.2 g of compound B), 2,3,4,5-tetraiodopyrrol-1-acetic acid ethyl ester (35.32 mmol) , in 840 mL of a dioxane (750 mL) / H2O (90 mL) mixture, 36 mL of 1M NaOH (36 mmol) are quickly added (10 min) and the final solution is kept at room temperature for 4 h. The reaction mixture is treated with carbon Carbopuron 4N, filtered, then acidified with 37% HC1 (w/w) and diluted in 500 1 of H2O, to give a solid which is filtered and purified by chromatography (silica gel (product E. Merck item 9385): eluent: CHCl3 : MeOH : 25% NH4OH (w/w) =7.5:2:0.3 (v/v/v)). Fractions with similar purity are collected, evaporated and diluted with 200 mL of H2O. By acidifying the aqueous phase with 40 mL of 1M HCl , a solid precipitates, which is filtered, washed with H2O and dried under reduced pressure. 21.5 g of 2,3,4,5-tetraiodopyrrol-1-acetic acid(34.20 mmol) are obtained.

1. additionThe reaction mixture is treated with carbon Carbopuron 4N
2. filtrationfiltered
3. additiondiluted in 500 1 of H2O
4. customto give a solid which
5. filtrationis filtered
6. custompurified by chromatography (silica gel (product E. Merck item 9385): eluent: CHCl3 : MeOH : 25% NH4OH (w/w) =7.5:2:0.3 (v/v/v))
7. customFractions with similar purity are collected
8. customevaporated
9. additiondiluted with 200 mL of H2O
10. customa solid precipitates
11. filtrationwhich is filtered
12. washwashed with H2O
13. customdried under reduced pressure