反応 #1509609

反応方程式

compound

5-(1,3-Dioxo-1,3-dihydroisoindol-2-yl)-2-(4,7,10-trisethoxycarbonylmethyl-1,4,7,10-tetraazacyclododec-1-yl)pentanoic acid benzyl ester

→

product

収率 138.3%

5-Amino-2-(4,7,10-triscarboxymethyl-1,4,7,10-tetraazacyclododec-1yl)pentanoic acid

収率 138.3%

溶媒

hydrochloric acid

反応条件

後処理

1. 1
   温度After cooling
2. 2
   ろ過filtration
3. 3
   濃縮the filtrate is concentrated
4. 4
   その他purified over silanized silica (elution with water)
5. 5
   その他After evaporation under reduced pressure
6. 6
   洗浄the product is washed with ether

実験手順

A solution of 54 g of compound obtained in stage 2 (64 ml) in 37% hydrochloric acid (1.81) is refluxed overnight in a 5-liter reactor. After cooling and filtration, the filtrate is concentrated and purified over silanized silica (elution with water). After evaporation under reduced pressure, the product is washed with ether. 45 g of product are obtained in the form of a white solid. The product is desalified by passing it over OH resin. 30 g of product are isolated in the form of white crystals (yield 100%).

出典