تفاعل #320606

معادلة التفاعل

N-methoxyacetyl-5-methylamino-2,4,6-triiodoisophthalic acid dichloride

iminodiacetic acid diethyl ester hydrochloride

triethylamine

N,N-dimethylformamide

→

N-Methoxyacetyl-5-methylamino-2,4,6-triiodoisophthalic acid-N,N-bis-(ethoxycarbonylmethyl)-amide-chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىA suspension results
2. 2
   تركيزThen, it is concentrated by evaporation
3. 3
   أخرىthe residue is chromatographed on silica gel 60 (Merck) with dichloromethane/ethyl acetate
4. 4
   تركيزAfter concentration
5. 5
   أخرىby evaporation of the product fractions
6. 6
   أخرىa colorless solid is obtained
7. 7
   أخرىwhich is dried in a vacuum

الإجراء التجريبي

A solution of 68.2 g (100 mmol) of N-methoxyacetyl-5-methylamino-2,4,6-triiodoisophthalic acid dichloride (EP 0015867) in 500 ml of N,N-dimethylformamide is mixed with 22.6 g (100 mmol) of iminodiacetic acid diethyl ester hydrochloride (production according to Jongkees, Recl. Trav. Chimys-Bas, 27, 296 (1908)) and 10.1 g (100 mmol) of triethylamine. A suspension results, which is stirred overnight under argon at room temperature. Then, it is concentrated by evaporation and the residue is chromatographed on silica gel 60 (Merck) with dichloromethane/ethyl acetate. After concentration by evaporation of the product fractions, a colorless solid is obtained, which is dried in a vacuum.

المصدر