反応 #11168

反応方程式

(2,6-dichloro-3-methoxyphenyl)methanol

HBr

bromide

triphenylphosphine

→

phosphonium

収率 97.0%

(2,6-Dichloro-3-methoxybenzyl)(triphenyl)phosphonium bromide

収率 97.0%

溶媒

acetic acid

CH2Cl2 benzene

反応条件

実験手順

Bromination of (2,6-dichloro-3-methoxyphenyl)methanol with 30% HBr in acetic acid, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 112, except that the reaction time for the displacement was 36 h, gave the phosphonium salt (526) (97%) as a white solid, mp (CH2Cl2/benzene) 242–244° C. 1H NMR (CDCl3) δ 7.83–7.60 (m, 15H), 7.15 (dd, J=9.1, 0.8 Hz, 1H), 6.88 (dd, J=9.0, 2.4 Hz, 1H), 5.41 (d, J=14.3 Hz, 2H), 3.84 (s, 3H). Found: C, 58.68; H, 4.16. C26H22BrCl2OP requires C, 58.67; H, 4.17.

出典