ChemicalBook CAS DataBase List AKOS B013927

AKOS B013927 synthesis

6synthesis methods

Product Name:AKOS B013927
CAS Number:7472-69-7
Molecular formula:C10H11BrO3
Molecular Weight:259.1

106-41-2
496 suppliers
$13.00/5g

67-66-3 Synthesis

67-66-3
6 suppliers
$39.79/500ml

67-64-1
6 suppliers
$21.60/10ml

7472-69-7
31 suppliers
$57.50/250mg

Yield:7472-69-7 91%

Reaction Conditions:

Stage #1: 4-bromo-phenol;chloroform;acetonewith sodium hydroxide at 20 - 35; for 21.5 h;Heating / reflux;
Stage #2: with hydrogenchloride in water at 0;

Steps:

28.a

Finely crushed NaOH pellets (23.0 g, 576 mmol) were added in portions to 4-bromophenol (10.4 g, 60 mmol) in acetone (146 mL, 1980 mmol) keeping the temperature below 28°C. CHC13 (13 mL, 161 mmol) ) was added dropwise keeping the temperature below 35°C and the mixture was stirred at that temperature for 30 min, then at reflux for 3 h and at room temperature for 18 h. The mixture was then concentrated and the residue was diluted with water, cooled in an ice-bath and acidified with HCl (6M). The precipitate was allowed to settle and was collected by decantation. Water was added to the solid and the mixture was stirred vigorously for 5 min and then filtered. The solid was dried to give the -sub-title compound (14.0 g; 91%).

References:

WO2005/123673,2005,A1 Location in patent:Page/Page column 61