1,3-Dibromobenzene → HCID 54317339, Verbindung

A mixture of 4-acetyl-2-nitroaniline (3.41 g, 18.94 mmol), 1,3-dibromobenzene (4.6 ml, 38.06 mmol), potassium carbonate (2.62 g, 19 mmol) and a catalytic amount of copper bronze is heated with stirring to 180° C. under a stream of nitrogen for 2 days. After cooling the solid reaction cake is extracted with a mixture of dichloromethane and methanol (9:1). The extract is concentrated under reduced pressure. The residue is extracted with ethyl acetate. This extract is concentrated under reduced pressure and the residue is eluted through silica gel with a mixture of petroleum ether and ethyl acetate (4:1) to afford the pure product. Yield 0.67 g (10.6%). Mp. 142-144° C.

1. temperatureAfter cooling
2. customthe solid reaction cake
3. extractionis extracted with a mixture of dichloromethane and methanol (9:1)
4. concentrationThe extract is concentrated under reduced pressure
5. extractionThe residue is extracted with ethyl acetate
6. concentrationThis extract is concentrated under reduced pressure
7. washthe residue is eluted through silica gel with a mixture of petroleum ether and ethyl acetate (4:1)
8. customto afford the pure product

ORD-Eintrag

ord-89337d7dbf0042e6a31750e6bbde88a5

Quelldatensatz

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05922725