反应详情

840 ml (6.1 Mol) triethylamine is added to a solution of 759 g (1.2 Mol) 3,5-diacetamido-2,4,6-triiodobenzoyl chloride and 276 g (1.8 Mol) sarcosine ethyl ester hydrochloride in 7600 ml N,N-dimethylformamide and stirred for 1 hr. at 60° C. The reaction mixture is cooled to room temperature, the crystallized triethyl ammonium chloride is filtered, washed with N,N-dimethylformamide and reduced under vacuum in a rotary evaporator. The residue is dissolved in 650 ml methanol and added dropwise to 3 l ethyl acetate. The precipitate is crystallized overnight, filtered to a dry state and finally washed with water, 1N hydrochloric acid, cold saturated sodium bicarbonate, water and dried under vacuum at 60° C. Yield: 685 g (80%).

1. customat 60° C
2. filtrationthe crystallized triethyl ammonium chloride is filtered
3. washwashed with N,N-dimethylformamide
4. customreduced under vacuum in a rotary evaporator
5. dissolutionThe residue is dissolved in 650 ml methanol
6. additionadded dropwise to 3 l ethyl acetate
7. customThe precipitate is crystallized overnight
8. filtrationfiltered to a dry state
9. washfinally washed with water, 1N hydrochloric acid, cold saturated sodium bicarbonate, water
10. customdried under vacuum at 60° C