Reaktion #2078552

Reaktionsgleichung

3-Bromo-5-tert-butyl-N-(2-chloro-4-nitro-phenyl)-6-hydroxy-2-methyl-benzamide

sodium carbonate

→

5-tert-Butyl-4-hydroxy-2-methyl-biphenyl-3-carboxylic acid (2-chloro-4-nitro-phenyl)amide

Lösungsmittel

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was evaporated
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   Waschenthe organic phase was washed with citric acid solution (10%)
4. 4
   TrocknenThe organic phase was dried over sodium sulphate
5. 5
   Sonstigeevaporated
6. 6
   SonstigeThe crude compound was purified by column chromatography

Vorschrift

To a solution of 3-Bromo-5-tert-butyl-N-(2-chloro-4-nitro-phenyl)-6-hydroxy-2-methyl-benzamide (0.18 g, 0.4 mmole) in dioxane (5 ml) under nitrogen phenylboronic acid (50.0 mg, 0.4 mmole), tetrakis(triphenylphosphine)palladium(0) (10 mg, 0.009 mmole) and sodium carbonate (1.41 ml, 2 M solution in water) were added. The reaction mixture was heated at 100° C. for 6 hours. The reaction mixture was evaporated, diluted with ethyl acetate and the organic phase was washed with citric acid solution (10%). The organic phase was dried over sodium sulphate and evaporated. The crude compound was purified by column chromatography.

Quelle