Реакция #521306

ord-cd05c9f4b3ae4e5b8767e3ad1334e93a

Реагенты

Нет

Условия реакции

Температура
100°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеcan be performed in a gravity bed reactor
  2. 2
    Другоеequipped with paddle stirring
  3. 3
    workup.ADDITIONto disperse the solid
  4. 4
    ДругоеThe excess borane can be removed by conventional distillation

Методика

The reaction of equation (10) is exothermic. For example, this reaction can be performed in a gravity bed reactor 190, as illustrated in FIG. 1. In such an apparatus, excess liquid triethyl borate can be added to solid sodium hydride in a reactor equipped with paddle stirring. The mixture can be maintained at a temperature from about 0° C. and about 100° C., preferably from about 60° to about 70° C., for about 1 to about 24 hours, preferably from about 1 to about 6 hours, with stirring to disperse the solid. The excess borane can be removed by conventional distillation, not shown, to give solid sodium triethoxyborohydride in quantitative yield.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06670444B2uspto-grants-2003_12