반응 #219173

반응 방정식

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

title compound 1a

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

bromoacetyl bromide

→

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

용매

dimethylacetamide

반응 조건

후처리

1. 1
   여과the accumulating solid 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

50 g (76.1 mmol) of N,N-bis-(2-aminoethyl)-5-(methylamino)-2,4,6-triiodoisophthalic acid amide (title compound 1a) is dissolved in 500 ml of dimethylacetamide, and at 0° C., 70.6 g (350 mmol) of bromoacetyl bromide (Aldrich) is added in drops over 15 minutes. 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.

출처