Réaction #4057

ord-71c80b666f9146bca8517cd2a6af9e46

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrea 2 h reaction time at room temperature
  2. 2
    Températureof heating
  3. 3
    Températureat reflux

Mode opératoire

The procedure of Example 1 was followed except that triethylphosphate (3.4 mL, 20 mmol) was added by syringe to a slurry of potassium trimethylsilanolate (2.56 g, 20 mmol) in dry tetrahydrofuran (50 mL), and a 2 h reaction time at room temperature was used, followed by 40 h of heating at reflux. Potassium diethylphosphate (3.55 g, 92% yield) was isolated as a white solid: 1H NMR (D2O, DSS) δ 1.1 (t, J=6.9 Hz, 6H), 3.75 (q, J=6.9 Hz, 4H). Anal. Calcd. for C4H10KO4P: C, 25.00; H, 5.24; K, 20.34. Found: C, 25.83, 25.88; H, 5.40, 5.29; K, 20.37, 20.10.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04723016uspto-grants-1988_02