Reaktion #1509612

Reaktionsgleichung

compound

2-(6,9-Bisethoxycarbonylmethyl-3,6,9,15-tetraazabicyclo[9.3.1]pentadeca-1(15),11,13-trien-3-yl)pentanedioic acid diethyl ester

sodium hydroxide

→

2-(6,9-Biscarboxymethyl-3,6,9,15-tetraazabicyclo[9.3.1]pentadeca-1(15),11,13-trien-3-yl)pentanedioic acid

Ausbeute 60.0%

Lösungsmittel

water

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for 24 h
2. 2
   workup.ADDITIONby adding weakly acidic resin
3. 3
   FiltrationThe resin is filtered off
4. 4
   Waschenwashed with water
5. 5
   workup.ADDITIONA strongly basic resin is added to the filtrate
6. 6
   Filtrationfiltered off
7. 7
   Waschenwashed twice with water
8. 8
   WaschenThe product is eluted with 50% acetic acid
9. 9
   SonstigeAfter evaporation to dryness
10. 10
    Sonstigethe product is obtained in the form of brown crystals

Vorschrift

15 mg of the compound obtained in stage 2 (26.5 μmol) are dissolved in 40 μl of ethanol and 53 μl of 5N sodium hydroxide are added dropwise rapidly. The mixture is brought to reflux for 24 h. The reaction medium is diluted 10-fold with water and the pH is then adjusted to 6.5 by adding weakly acidic resin. The resin is filtered off and washed with water. A strongly basic resin is added to the filtrate and then filtered off and washed twice with water. The product is eluted with 50% acetic acid. After evaporation to dryness, the product is obtained in the form of brown crystals. m=8 mg. Yield=60%.

Quelle