反応 #318466

ord-e17e630651bc4823b01a22b74fce5162

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    その他to obtain a uniform mixture
  3. 3
    温度Thereafter, the reaction system was cooled down to room temperature, to which
  4. 4
    その他The resultant NaCl precipitate was removed by filtration
  5. 5
    workup.DISTILLATIONthe ethanol was distilled off under reduced pressure

実験手順

50 g (0.19 mol) of sodium butyl 2-hydroxy-3chloropropyl phosphate was charged into a reactor, to which 1000 ml of ethanol was added, followed by agitation and heating to 70° C. to obtain a uniform mixture. Thereafter, the reaction system was cooled down to room temperature, to which was gradually added 88.6 g (0.19 mol) of a 0.0021 mol/g sodium hydroxide ethanol solution, followed by agitation for 3 hours while keeping the temperature. The HPLC analysis revealed the disappearance of a peak of the starting material with a peak for the resultant new product appearing. The resultant NaCl precipitate was removed by filtration and the ethanol was distilled off under reduced pressure to obtain 43 g (yield: 100%) of sodium butyl glycidyl phosphate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04845239uspto-grants-1989_07