تفاعل #487557

ord-99e333eb388c4b31b9b81b7e8ce74091

معادلة التفاعل

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
المردود 100.0%

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONis added anhydrous chloroform (6 ml)
  3. 3
    درجة الحرارةthe suspension is heated at this temperature for 5 hours
  4. 4
    درجة الحرارةThe mixture is then cooled to room temperature
  5. 5
    تركيزconcentrated to a small volume
  6. 6
    أخرىtriturated with hexanes
  7. 7
    ترشيحfiltered

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08741806B2uspto-grants-2014_06