the synthesis process is as follows:
n-bromosuccinmide; dibenzoyl peroxide; dimethyl amine; tetrachloromethane; water;
reactants are commercially availlable.
benarous, richard, wo2012/140243, a1, (2012) to a solution of methyl 2-bromo-3-methylbenzoate (28a) (3.35 g, 15.0 mmol) in carbon tetrachloride (35 ml) were added a/-bromosuccinimide (5.20 g, 29 mmol) and benzoyl peroxide (363 mg, 1 .5 mmol). the mixture was degassed for 15 minutes an d refluxed overnight. the mixture was filtered and the filtrate was concentrated in vacuo. the residue was dissolved in 40percent dimethylamine (46 ml) and irradiated (200w) for 15 minutes at 60°c. the solution was extracted with dichlorome thane (2x30 ml). the organic layers were dried over sodium sulfate and concentrated in vacuo to provide methyl 2-bromo-3-formylbenzoate (28b) (2.12 g, 8.72 mmol, 58percent) as a white solid.1 h nmr (400 mhz, cdci3) 3.97 (s, 3h), 7.49 (t, j = 8.0 hz, 1 h), 7.89 (dd, j = 1 .0 hz, j= 8.0 hz, 1 h), 8.00 (dd, j = 1 .0 hz, j= 8.0 hz, 1 h), 10.49 (s, 1 h).
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