반응 #487557

ord-99e333eb388c4b31b9b81b7e8ce74091

반응 방정식

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
수율 100.0%

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타thoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONis added anhydrous chloroform (6 ml)
  3. 3
    온도the suspension is heated at this temperature for 5 hours
  4. 4
    온도The mixture is then cooled to room temperature
  5. 5
    농축concentrated to a small volume
  6. 6
    기타triturated with hexanes
  7. 7
    여과filtered

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08741806B2uspto-grants-2014_06