2-BROMO-1-(3,5-DICHLORO-2-METHOXYPHENYL)ETHANONE synthesis

Yield:-

Reaction Conditions:

Stage #1: 2-bromo-1-(3,5-dichloro-2-methoxy-phenyl)-ethanone;thiourea in ethanol at 165; for 0.0833333 h;Microwave iiradiation;
Stage #2: with sodium hydroxide in water; pH=7;

Steps:

2.A

2-Bromo-1-(3,5-dichloro-2-methoxy-phenyl)-ethanone (200 mg, 0.746 mmol), thio-urea (100 mg, 1.3 mmol) in ethanol (2 mL) and heated to 165° C. for 300 s in a Emrys optimizer EXP microwave. The volatile solvent was removed and the residue dissolved in water and adjusted to pH 7 with sodium hydroxide. The aqueous mixture was extracted with ethyl acetate (3×50 mL), and evaporated to dryness to give a oily residue. This was then used without further purification in the next step.

References:

US2007/105920,2007,A1 Location in patent:Page/Page column 4