Carbonochloridic acid, 4-bromo-2-methoxyphenyl ester synthesis

Yield:1169939-54-1 77%

Reaction Conditions:

with N,N-dimethyl-aniline in toluene at 0 - 20; for 3.5 h;

Steps:

4.a

To an ice-cooled stirred solution of 4-bromo-2-methoxyphenol (4.06 g, 20 mmol) and phosgene (11.58 mL, 22.00 mmol) was added dropwise N,N-dimethylaniline (2.424 g, 20.00 mmol) dissolved in Toluene (9 mL). The reaction was stirred at room temperature for 3 hours. Whereupon nitrogen was bubbled through the reaction mixture for 30 min; and quenched with ice. The organic phase was washed with IN HCl solution and water respectively. After drying over MgSO₄ toluene was removed by vacuum and 4-bromo-2- methoxyphenyl carbonochloridate was obtained as oil. Yield: 4.1O g, 77%.

References:

WO2009/84970,2009,A1 Location in patent:Page/Page column 65