diisobutylaluminium hydride; hydrogenchloride; tetrahydrofuran; hexanes; dichloromethane; tetrahydrofuran; methanol; hexanes; dichloromethane; water;
reactants are commercially availlable.
glaxo group limited, wo2007/65669, a1, (2007) ethyl 2-bromothiazole-4-carboxylate (3g, 12.7mmol) was taken up in thf and dichloromethane (100ml each) and cooled to -780c. 1 m dibal-h in hexanes (25.4ml, 25.4mmol) was added dropwise maintaining the temperature at <-70°c. the solution wa s stirred for 5h and quenched with meoh (20ml). the solution was allowed to warm to room temperature, poured into 1 m hci (200ml) and extracted with etoac (3x100ml). the combined organics were washed with brine (300ml), dried (na2so4) and c oncentrated. purification by column chromatography on silica (0-50percent etoac\\40-60 pet. ether gradient) yielded the product as a white solid (0.862g). deltah (cdci3) 8.10(1 h, s), 9.95(1 h, s).
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