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Beta-Alanine → Sodium butyl glycidyl phosphate

HRID 1460407
ノート
印刷プレビュー

反応式

HRID 1460407 の反応式
N[CH2:2][CH2:3][C:4](O)=O.O.[P:8]([O-:17])([O-:16])([O:10][CH2:11][CH:12]([OH:15])[CH2:13]Cl)=[O:9].[Na+:18].[Na+].[OH-].[Na+].[CH2:22](O)C>>[P:8]([O-:17])([O:10][CH2:11][CH:12]1[O:15][CH2:13]1)([O:16][CH2:4][CH2:3][CH2:2][CH3:22])=[O:9].[Na+:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 239Beta-AlanineHCID 702Ethanol2 回HCID 962WaterHCID 14798Sodium HydroxideHCID 12112254Sodium 2-hydroxy-3-chloropropyl phosphate

生成物 1

HCID 23698436Sodium butyl glycidyl phosphate収率 99.3%

反応条件

温度
70 °C

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%.

後処理

  1. additionwas added
  2. stirringthe mixture was homogenized
  3. temperatureThen, while maintaining the temperature
  4. customfollowed by purification
  5. additionwas added dropwise
  6. stirringstirring
  7. customThe reaction was terminated
  8. customUpon completion of the reaction
  9. customthe product was collected by fractionation by HPLC
  10. customThe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-daabaf86d1eb4c16a1308811fd99ac77
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05071585

反応ノート

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