반응 #219176

반응 방정식

N,N-bis-[2-(2-aminoacetylamino)ethyl]-5-(methylamino)-2,4,6-triiodoisophthalic acid amide

2-bromopropionic acid bromide

→

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

용매

dimethylacetamide

반응 조건

후처리

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

실험 절차

57.8 g (75 mmol) of N,N-bis-[2-(2-aminoacetylamino)ethyl]-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 solid that accumulates 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.

출처