反応 #219175

反応方程式

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

title compound 6a

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

bromoacetyl bromide

→

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

溶媒

dimethylacetamide

反応条件

後処理

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

実験手順

50 g (77.8 mmol) of N,N-bis-(2-aminoethyl)-5-amino-2,4,6-triiodoisophthalic acid amide (title compound 6a) is dissolved in 500 ml of dimethylacetamide, and 70.6 g (350 mmol) of bromoacetyl 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.

出典