反应 #500172

反应方程式

water

1.5-bis(2,6-dioxomorpholino)-3-carboxymethyl-3-azapentane

triethylamine

11-aminoundecanoic acid ethyl ester

→

title compound

3,6-Bis(carboxymethyl)-9-(10-carbethoxydecylcarbamoylmethyl)-3,6,9-triazaundecanedioic acid

溶剂

dimethylformamide

反应条件

后处理

1. 1
   温度The solution is heated for 3 hours to 70° C.
2. 2
   其他the solution is evaporated to dryness in a vacuum
3. 3
   workup.ADDITIONthe solution is mixed by drops with concentrated hydrochloric acid until permanent cloudiness
4. 4
   workup.STIRRINGAfter stirring overnight in the ice bath
5. 5
   洗涤washed with water
6. 6
   其他dried in a vacuum at 50° C

实验过程

17.85 g (50 mmol) of 1.5-bis(2,6-dioxomorpholino)-3-carboxymethyl-3-azapentane is stirred in 200 ml of dimethylformamide and mixed with 9 ml (50 mmol) of water. The solution is heated for 3 hours to 70° C., cooled off to 0° C. and 36.07 ml (260 mmol) of triethylamine and 10.8 g (50 mmol) of 11-aminoundecanoic acid ethyl ester are added. After stirring overnight at room temperature, the solution is evaporated to dryness in a vacuum. The residue is taken up in 100 ml of water and the solution is mixed by drops with concentrated hydrochloric acid until permanent cloudiness. After stirring overnight in the ice bath, the finely crystalline precipitate is suctioned off, washed with water and dried in a vacuum at 50° C. 14.9 g (65% of theory) of the title compound is obtained as a white powder with melting point 155-157° C.

来源