反应详情

7.75 g (50 mmol) of 2-amino-5-methoxy-thiophenol are dissolved in 150 ml methylene chloride and 14.1 g (70 mmol) of bromoacetylbromide are added whilst cooling with ice. Then the mixture is heated for 1 hour to reflux temperature. After cooling solid potassium carbonate is added until foaming ceases, the mixture is filtered and the filtrate is evaporated down. The evaporation residue is purified by column chromatography on neutral aluminium oxide (eluant: petroleum ether/ethyl acetate=3:1). Yield: 6.8 g (52.7 of theory), Melting point: 90-91° C.

1. temperaturewhilst cooling with ice
2. temperatureThen the mixture is heated for 1 hour
3. temperatureto reflux temperature
4. additionis added
5. filtrationthe mixture is filtered
6. customthe filtrate is evaporated down
7. customThe evaporation residue is purified by column chromatography on neutral aluminium oxide (eluant: petroleum ether/ethyl acetate=3:1)