Реакция #418001

ord-7abb273025a24a32a20970e1b100f87e

Уравнение реакции

COC(=O)C(C)(C)c1ccc(Br)cc1
2-(4-bromo-phenyl)-2-methyl-propionic acid methyl ester
[I-].[Na+]
sodium iodide
CNCCNC
N,N′-dimethylethylendiamine
COC(=O)C(C)(C)c1ccc(I)cc1
desired product
COC(=O)C(C)(C)c1ccc(I)cc1
2-(4-Iodo-phenyl)-2-methyl-propionic acid methyl ester

Растворители

Условия реакции

Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling
  2. 2
    Промывкаwashed with 5% ammonia and water
  3. 3
    СушкаThe organic layer is dried over sodium sulphate
  4. 4
    ДругоеThe solvent is evaporated

Методика

To 0.45 g (1.7 mmol) 2-(4-bromo-phenyl)-2-methyl-propionic acid methyl ester (WO2008/002671) in 1.5 mL 1,4-dioxane are added 34 mg (0.18 mmol) copper(I) iodide, 0.53 g (3.5 mmol) sodium iodide and 0.04 mL (0.35 mmol) N,N′-dimethylethylendiamine under inert gas atmosphere. The mixture is stirred at 110° C. for 12 h. After cooling, the mixture is diluted with EtOAc and washed with 5% ammonia and water. The organic layer is dried over sodium sulphate. The solvent is evaporated to yield the desired product.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08877754B2uspto-grants-2014_11