反应详情

温度

60 °C

A mixture of 2,5-dimethyl-4-nitroaniline (0.96 g), ferric chloride hexahydrate (2.50 g), zinc chloride (0.094 g), concentrated hydrochloric acid (0.481 mL), and ethanol (8 mL) is heated to 60° C. 1,3,3-trimethoxybutane (0.73 mL) is added dropwise while the reaction mixture is kept at 60° C. The reaction mixture is heated at reflux overnight and cooled to room temperature. A solution of 10% aqueous sodium hydroxide is added, and the mixture is extracted three times with methylene chloride. The combined organic layers are dried over sodium sulfate, filtered and evaporated to afford a crude product. The crude product is purified by flash chromatography using 25% ethyl acetate in hexane as eluent, providing 6-nitro-4,5,8-trimethylquinoline.

1. customis kept at 60° C
2. temperatureThe reaction mixture is heated
3. temperatureat reflux overnight
4. temperaturecooled to room temperature
5. extractionthe mixture is extracted three times with methylene chloride
6. dry with materialThe combined organic layers are dried over sodium sulfate
7. filtrationfiltered
8. customevaporated
9. customto afford a crude product
10. customThe crude product is purified by flash chromatography