反応 #790953

反応方程式

β-Alanine

water

sodium 2-hydroxy-3-chloropropyl phosphate

sodium hydroxide

ethanol

ethanol

→

sodium butyl glycidyl phosphate

収率 99.3%

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe mixture was homogenized
3. 3
   温度Then, while maintaining the temperature
4. 4
   その他followed by purification
5. 5
   workup.ADDITIONwas added dropwise
6. 6
   workup.STIRRINGstirring
7. 7
   その他The reaction was terminated
8. 8
   その他Upon completion of the reaction
9. 9
   その他the product was collected by fractionation by HPLC
10. 10
    その他The solvent was evaporated in vacuo

実験手順

β-Alanine, 30.0 g (0.337 mol), was charged into a reaction vessel, into which 100 ml of water was added and the mixture was stirred. Its temperature was raised to 70° C. and the mixture was homogenized. Then, while maintaining the temperature, an ethanol solution of 750 g (0.112 mol) of sodium butyl glycidyl phosphate, which was prepared by the reaction of 30.2 g (0.112 mol) of sodium 2-hydroxy-3-chloropropyl phosphate and sodium hydroxide in ethanol, followed by purification by desalting, was added dropwise, and stirring was continued for further 6 hours. The reaction was terminated, when the analysis by HPLC indicated extinction of the peak for the raw material and appearance of the peak for the new product. Upon completion of the reaction, the product was collected by fractionation by HPLC. The solvent was evaporated in vacuo to produce 35.8 g of sodium 2-hydroxy-3-N-carboxyethylammoniopropyl phosphate at a yield of 99.3%.

出典