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psyloxy
(Hive Addict) 09-23-03 22:51 No 460610 |
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2,5-diMeOPhMeBr from 2,5-diMeOPhMe/NBS - 99% yield | Bookmark | |||||
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-- |
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