2-BROMO-1-(2,6-DIMETHOXYPHENYL)ETHANONE synthesis

Yield:123184-19-0 70%

Reaction Conditions:

with phenyltrimethylammonium tribromide in tetrahydrofuran at 20; for 1.16667 h;

Steps:

C.14

(C-14) To a solution of the above-mentioned compound C-13 (4.0g, 22.2mmol) in tetrahydrofuran (40ml), was added phenyltrimethylammoniumtribromide (8.34g, 22.2mmol) over 10 minutes at room temperature and the mixture was stirred at the same temperature for 1 hour.. water was added thereto, and the mixture was extracted with ethyl acetate, washed, and dried, then the solvent was evaporated under reduced pressure.. The residue was purified with silica gel column chromatography (ethyl acetate:n-hexane=1:4).. After allowing to stand at room temperature, the obtained solid residue was washed with diisopropylether to give 2-bromo-1-(2,6-dimethoxyphenyl)etanone (4.22g yield: 70%). Melting point: 78-82°C NMR(CDCl3)δ: 3.82(6H, s), 4.38(2H, s), 6.57(2H, d, J=8.4Hz), 7.32(1H, t, J=8.4Hz).

References:

EP1422218,2004,A1 Location in patent:Page 188