反応 #487557

ord-99e333eb388c4b31b9b81b7e8ce74091

反応方程式

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
収率 100.0%

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他thoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONis added anhydrous chloroform (6 ml)
  3. 3
    温度the suspension is heated at this temperature for 5 hours
  4. 4
    温度The mixture is then cooled to room temperature
  5. 5
    濃縮concentrated to a small volume
  6. 6
    その他triturated with hexanes
  7. 7
    ろ過filtered

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08741806B2uspto-grants-2014_06