Author Topic: 2,5-diMeOPhMeBr from 2,5-diMeOPhMe/NBS - 99% yield  (Read 1652 times)

0 Members and 1 Guest are viewing this topic.

psyloxy

  • Guest
2,5-diMeOPhMeBr from 2,5-diMeOPhMe/NBS - 99% yield
« on: September 23, 2003, 10:51:00 PM »
2,5-Dimethoxybenzyl Bromide

In a dry 2-neck 250ml rb flask equipped with a reflux condenser, mag stirring bar, and a N2 inlet was placed 2,5-dimethoxytoluene (10g 0.066 mol). To the flask was added 180ml of CCl4, NBS (17.77g 0.099mol) and a catalytic amount of benzoyl peroxide. The reaction mixture was refluxed for 2h and checked by TLC. The succinimide was filtered off, and the resulting solution was concentrated on a rotovap. The yellow liquid was crystallized from hexane. The product was obtained as a yellow solid and was used without any further purification: yield: 15.2g (99.2%)

Ref: Bae, I. T.; Sandifer, M.; Le, Y. W.; Tryk, D. A.; Sukenuk, C. N.; Scherson, D. A.;ANCHAM; Anal.Chem.; 67; 24; 1995; 4508-4513.

--psyloxy--