反应详情

温度

0 °C

6.85 g (10 mMol) N-(3,5-diacetamido-2,4,6-triiodobenzoyl)-sarcosine and 1.7 g (12.2 mMol) o-nitrophenol are dissolved in 15 ml N,N-dimethylformamide. 60 ml tetrahydrofuran is added to this solution which is then cooled down to 0° C. 2,5 g (12 mMol) N,N-dicyclohexylcarbodiimide is added. The reaction runs for 2 hours at 0° C. and overnight at room temperature. The precipitate (N,N'-dicyclohexylurea) is filtered off, washed with 10 ml N,N-dimethylformamide, the tetrahydrofuran is distilled, the solution kept in the refrigerator overnight and then the dicyclohexylurea is again filtered off. The organic solution is added dropwise to 250 ml ether, the precipitate is decantered, dissolved with 25 ml N,N-dimethylformamide and added to water dropwise. The precipitate is filtered, washed with saturated sodium bicarbonate solution and water and dried. Yield: 5.4 g (67%).

1. filtrationThe precipitate (N,N'-dicyclohexylurea) is filtered off
2. washwashed with 10 ml N,N-dimethylformamide
3. distillationthe tetrahydrofuran is distilled
4. customkept in the refrigerator overnight
5. filtrationthe dicyclohexylurea is again filtered off
6. additionThe organic solution is added dropwise to 250 ml ether
7. dissolutiondissolved with 25 ml N,N-dimethylformamide
8. additionadded to water dropwise
9. filtrationThe precipitate is filtered
10. washwashed with saturated sodium bicarbonate solution and water
11. customdried