Реакция #487557

ord-99e333eb388c4b31b9b81b7e8ce74091

Уравнение реакции

CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Pb+4]
lead tetraacetate
CCc1ccc(-c2ccc(Cl)cc2)cc1B(O)O
4′-chloro-4-ethylbiphen-3-ylboronic acid
CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CCc1ccc(-c2ccc(Cl)cc2)c[c]1[Pb+3]
4′-chloro-4-ethylbiphen-3-yllead triacetate
Выход 100.0%

Условия реакции

Температура
40°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONis added anhydrous chloroform (6 ml)
  3. 3
    Температураthe suspension is heated at this temperature for 5 hours
  4. 4
    ТемператураThe mixture is then cooled to room temperature
  5. 5
    Концентрированиеconcentrated to a small volume
  6. 6
    Другоеtriturated with hexanes
  7. 7
    Фильтрацияfiltered

Методика

To a mixture of lead tetraacetate (2.15 g, 4.85 mmol) and mercuric diacetate (0.15 g, 0.47 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (6 ml). This mixture is warmed to 40° C., and 4′-chloro-4-ethylbiphen-3-ylboronic acid (1.17 g, 4.50 mmol) is added in one portion and the suspension is heated at this temperature for 5 hours. The mixture is then cooled to room temperature, concentrated to a small volume and triturated with hexanes and filtered to yield crude 4′-chloro-4-ethylbiphen-3-yllead triacetate (2.70 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08741806B2uspto-grants-2014_06