反应详情

温度

-10 °C

A solution of 1-hydroxymethyl-2,3,4-trimethoxybenzene (1 g, 5 mmoles) in anhydrous ethered solution (10 ml) is injected into a three-necked flask supplied with a septum and equipped with a magnetic stirrer, which is swept with argon. Phosphorus tribromide at -20° C. (1.46 g, 5 mmoles) dissolved in ether (8 ml) is then added. The mixture is stirred at -10° C. for 2 hours and then washed with ice-cold water and finally with NaCl, and then dried over MgSO4. Evaporation at 0° C. under reduced pressure gives a colorless oil (1.24 g) which is homogeneous in TLC (Y=95%).

1. customequipped with a magnetic stirrer
2. additionis then added
3. washwashed with ice-cold water and finally with NaCl
4. dry with materialdried over MgSO4
5. customEvaporation at 0° C. under reduced pressure