반응 #1509612

반응 방정식

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

수율 60.0%

용매

water

ethanol

반응 조건

후처리

1. 1
   온도to reflux for 24 h
2. 2
   workup.ADDITIONby adding weakly acidic resin
3. 3
   여과The resin is filtered off
4. 4
   세척washed with water
5. 5
   workup.ADDITIONA strongly basic resin is added to the filtrate
6. 6
   여과filtered off
7. 7
   세척washed twice with water
8. 8
   세척The product is eluted with 50% acetic acid
9. 9
   기타After evaporation to dryness
10. 10
    기타the product is obtained in the form of brown crystals

실험 절차

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%.

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