Trimethyl phosphite → HCID 21805256, compound

Participants

Reaction Steps

8.8 g of trimethyl phosphite are added to 20.0 g of 3-bromo-2-hydroxy-5-methoxy-benzyl bromide and, with stirring, the mixture is heated for 3 hours at 140° (complete conversion according to TLC). The resulting oil is filtered with toluene/ethyl acetate (4:1) as eluant over a small amount of silica gel. [(3-Bromo-2-hydroxy-5-methoxy-phenyl)methyl ]phosphonic acid dimethyl ester is thus obtained [1H-NMR (360 MHz, CDCl3); 3.20 (d, 2H, CH2P, 2JP-H =21 Hz), 3.70 (s, 3H, OCH3), 3.74 (d, 6H, 2×OCH3,3JP-H =1 Hz), 6.70 (m, 1H), 7.07 (m, 1H) ppm].

Provenance & Evidence