تفاعل #219172

معادلة التفاعل

N,N-bis-(2-aminoethyl)-5-(methylamino)-2,4,6-triiodoisophthalic acid amide

2-bromopropionic acid bromide

→

N,N-Bis-[2-(2-bromopropionylamino)ethyl)-5-[(2-bromopropionyl)methylamino]-2,4,6-triiodoisophthalic acid amide

المذيبات

dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe accumulating solid is filtered off
2. 2
   workup.DISSOLUTIONdissolved in 800 ml of ethyl acetate
3. 3
   استخلاصextracted three times with 250 ml each of water
4. 4
   أخرىThe organic phase is dried on sodium sulfate
5. 5
   أخرىthe solvent is evaporated to the dry state
6. 6
   أخرىThe crude product is recrystallized from methyl-tert-butyl ether

الإجراء التجريبي

50 g (76.1 mmol) of N,N-bis-(2-aminoethyl)-5-(methylamino)-2,4,6-triiodoisophthalic acid amide is dissolved in 500 ml of dimethylacetamide, and 75.5 g (350 mmol) of 2-bromopropionic acid bromide (Aldrich) is added in drops over 15 minutes at 0° C. Then, it is stirred for 20 hours at 40° C. The reaction mixture is poured into 4000 ml of ice water, the accumulating solid is filtered off, dissolved in 800 ml of ethyl acetate and extracted three times with 250 ml each of water. The organic phase is dried on sodium sulfate, and the solvent is evaporated to the dry state. The crude product is recrystallized from methyl-tert-butyl ether.

المصدر