* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With potassium hydroxide;tetrabutylammomium bromide; In tetramethylurea; at 20℃; for 24h;
3,5-Dibromonitrobenzene (21.07 g, 75 mmol), freshly powdered potassium hydroxide (7.57 g, 135 mmol) and tetrabutylammonium bromide (2.42 g, 7.5 mmol) were suspended in tetramethyl urea (80 mL). To the resulting brown slurry was slowly added a solution of methanol (4.81 g, 6.09 mL, 150 mmol) in 20 mL of tetramethyl urea at room temperature over a period of 15 minutes. The mixture was stirred for 24 hours at room temperature then poured on ice (150 g) and was extracted with t-butyl methyl ether (3.x.250 mL). The combined organics were dried over magnesium sulfate and concentrated to give the crude product which was distilled (124° C., 10 Torr) to provide 16.74 g (84percent) of 3,5-dibromoanisole as a pale yellow solid.
84%
With potassium hydroxide; tetrabutylammomium bromide; tetramethylurea; at 20℃; for 24.25h;
(a) 3,5-Dibromoanisole. 3,5-Dibromonitrobenzene (21.07 g, 75 mmol), freshly powdered potassium hydroxide (7.57 g, 135 mmol) and tetrabutylammonium bromide (2.42 g, 7.5 mmol) were suspended in tetramethyl urea (80 mL). To the resulting brown slurry was slowly added a solution of methanol (4.81 g, 6.09 mL, 150 mmol) in 20 mL of tetramethyl urea at room temperature over a period of 15 minutes. The mixture was stirred for 24 hours at room temperature then poured on ice (150 g) and was extracted with t-butyl methyl ether (3.x.250 mL). The combined organics were dried over magnesium sulfate and concentrated to give the crude product which was distilled (124° C., 10 Torr) to provide 16.74 g (84percent) of 3,5-dibromoanisole as a pale yellow solid.
84%
With potassium hydroxide; tetrabutylammomium bromide; In tetramethylurea; at 20℃; for 24.25h;
0294] (a) 3,5-Dibromoanisole. 3,5-Dibromonitrobenzene (21.07 g, 75 mmol), freshly powdered potassium hydroxide (7.57g, 135 mmol) and tetrabutylammonium bromide (2.42 g, 7.5 mmol) were suspended in tetramethyl urea (80 mL). To the resulting brown slurry was slowly added a solution of methanol (4.81 g, 6.09 mL, 150 mmol) in 20 mL of tetramethyl urea at room temperature over a period of 15 minutes. The mixture was stirred for 24 hours at room temperature then poured on ice (150 g) and was extracted with t-butyl methyl ether (3x250 mL). The combined organics were dried over magnesium sulfate and concentrated to give the crude product which was distilled (1240C, 10 Torr) to provide 16.74 g (84percent) of 3,5- dibromoanisole as a pale yellow solid.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
