反应详情

A stirred suspension of 11.28 g of N-[2-[2-methylamino-2-(2-thienyl)ethyl]phenyl]-2,2-dimethylpropanamide in 100 ml of 6N hydrochloric acid was refluxed under nitrogen for 8 hours. The mixture was cooled, decanted over crushed ice and water (200 ml), basified by the addition of 50% sodium hydroxide solution, and extracted with dichloromethane (3×150 ml). The combined extract was dried over anhydrous sodium sulfate, filtered, and concentrated to an oil. The oil was purified by means of HPLC on a Water's Model 500A High Pressure Liquid Chromatograph (silica gel) utilizing methanol as the eluent. Concentration of the appropriate fractions yielded 5.96 g of 2-amino-N-methyl-α-(2-thienyl)benzeneethanamine. A sample of the product (2 g) in methanol (5 ml) was treated with ethereal hydrogen chloride and a solid was precipitated by further dilution with anhydrous ether. Recrystallization from absolute ethanol gave 2.12 g of 2-amino-N-methyl-α-(2-thienyl)benzeneethanamine dihydrochloride hemihydrate, mp 210°-215° C. (dec.).

1. temperaturewas refluxed under nitrogen for 8 hours
2. temperatureThe mixture was cooled
3. customdecanted
4. customover crushed ice and water (200 ml)
5. additionbasified by the addition of 50% sodium hydroxide solution
6. extractionextracted with dichloromethane (3×150 ml)
7. extractionThe combined extract
8. dry with materialwas dried over anhydrous sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated to an oil
11. customThe oil was purified by means of HPLC on a Water's Model 500A High Pressure Liquid Chromatograph (silica gel)