反应详情

A mixture of 20 g of (3-bromothien-2-yl) (3-methoxyphenyl)methanone and 17 g of methyl hydrazine in 134 ml of ethylene glycol was stirred under nitrogen at 120°-130° C. The reaction was complete in 2.5 hours. The product was allowed to cool to room temperature, and thereafter quenched with water (200 ml) and extracted with ether (4×200 ml). The organics were dried over anhydrous magnesium sulfate and the solvents were evaporated to give an oil. The oil was purified by HPLC (3:1 hexane/ethyl acetate). This yielded 9 g of a solid which was recrystallized from ether to give 8.2 g of crystals, mp 99°-101° C.

1. customquenched with water (200 ml)
2. extractionextracted with ether (4×200 ml)
3. dry with materialThe organics were dried over anhydrous magnesium sulfate
4. customthe solvents were evaporated
5. customto give an oil
6. customThe oil was purified by HPLC (3:1 hexane/ethyl acetate)
7. customThis yielded 9 g of a solid which was recrystallized from ether