反応 #1509612

反応方程式

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

収率 60.0%

溶媒

water

ethanol

反応条件

後処理

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

実験手順

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%.

出典