反应详情

A stirred solution of 5.02 g of 2-amino-N-methyl-α-(3-methyl-2-thienyl)benzeneethanamine and 79 ml of dimethylformamide was treated with a solution of 4.71 g N-bromosuccinimide in 55 ml of dimethylformamide. The solution was stirred for 8 h with the exclusion of moisture and then concentrated to an oil on a rotary evaporator (70° C.) under high vacuum. The oil was diluted with distilled water (100 ml) and basified with a 10% sodium hydroxide solution (25 ml). The basic solution was extracted with dichloromethane (3×100 ml). The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated to an oil. Thin layer chromatography (silica gel, methanol eluent) indicated a 2-component mixture.

1. concentrationconcentrated to an oil on a rotary evaporator (70° C.) under high vacuum
2. additionThe oil was diluted with distilled water (100 ml)
3. extractionThe basic solution was extracted with dichloromethane (3×100 ml)
4. dry with materialThe organic phase was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to an oil