Реакция #68756

ord-7a0a3d5313034f89b09bb452f512b217

Уравнение реакции

CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Pb+2]
lead(IV)acetate
OB(O)c1cc(Br)ccc1C1CC1
5-bromo-2-cyclopropylphenyl boronic acid
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Brc1ccc(C2CC2)[c]([Pb+3])c1.CC(=O)[O-].CC(=O)[O-].CC(=O)[O-]
5-bromo-2-cyclopropylphenyl lead triacetate

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураthe solution is heated at this temperature for 5 hours
  2. 2
    Температураis further cooled to 0° C.
  3. 3
    ФильтрацияThe reaction mixture is then filtered
  4. 4
    Промывка(washing with additional chloroform)
  5. 5
    Концентрированиеthe filtrate is concentrated to half its original volume
  6. 6
    Другоеthe crude product is precipitated with hexanes
  7. 7
    КонцентрированиеFurther concentration
  8. 8
    Фильтрацияfiltration

Методика

To a solution of lead(IV)acetate (4.0 g, 0.0089 mol) and mercury(II)acetate (139 mg, 0.45 mmol) in chloroform (12 ml) at 50° C. is added 5-bromo-2-cyclopropylphenyl boronic acid (2.0 g, 0.0083 mol), and the solution is heated at this temperature for 5 hours. After cooling to room temperature the suspension is further cooled to 0° C. and anhydrous potassium carbonate (1.8 g) is added with rapid stirring for 2 minutes. The reaction mixture is then filtered (washing with additional chloroform), and the filtrate is concentrated to half its original volume and the crude product is precipitated with hexanes. Further concentration then filtration affords 5-bromo-2-cyclopropylphenyl lead triacetate as a beige solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08530388B2uspto-grants-2013_09