反应 #1509612

反应方程式

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

收率 60.0%

溶剂

water

ethanol

反应条件

后处理

1. 1
   温度to reflux for 24 h
2. 2
   workup.ADDITIONby adding weakly acidic resin
3. 3
   过滤The resin is filtered off
4. 4
   洗涤washed with water
5. 5
   workup.ADDITIONA strongly basic resin is added to the filtrate
6. 6
   过滤filtered off
7. 7
   洗涤washed twice with water
8. 8
   洗涤The product is eluted with 50% acetic acid
9. 9
   其他After evaporation to dryness
10. 10
    其他the product is obtained in the form of brown crystals

实验过程

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%.

来源