Реакция #599764

ord-2660a104f465464fa90006c262d38d39

Уравнение реакции

CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Pb+4]
Lead tetraacetate
Cc1cc(OCc2ccccc2)cc(C)c1B(O)O
4-benzyloxy-2,6-dimethylphenyl boronic acid
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].Cc1cc(OCc2ccccc2)cc(C)[c]1[Pb+3]
4-benzyloxy-2,6-dimethylphenyl lead triacetate

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONChloroform (20 ml) is added
  3. 3
    ТемператураAfter further heating at 50° C. for 3 hours the reaction mixture
  4. 4
    Температураis cooled to 0° C.
  5. 5
    Фильтрацияbefore filtering
  6. 6
    Другоеevaporation of the crude solution under reduced pressure
  7. 7
    ДругоеThe crude product is then azeotroped with diethyl ether

Методика

Lead tetraacetate (5.7 g, 0.013 mol) and mercury (II) acetate (0.2 g, 0.0006 mol) are stirred together and thoroughly flushed with nitrogen. Chloroform (20 ml) is added and the dark orange solution heated to 50° C., followed by the addition of 4-benzyloxy-2,6-dimethylphenyl boronic acid (3 g, 0.012 mol) in one portion. After further heating at 50° C. for 3 hours the reaction mixture is cooled to 0° C. and potassium carbonate added (1.9 g, 0.02 mol). The suspension is stirred for just 5 minutes before filtering and evaporation of the crude solution under reduced pressure. The crude product is then azeotroped with diethyl ether to afford 4-benzyloxy-2,6-dimethylphenyl lead triacetate as a pale solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09102642B2uspto-grants-2015_08