反应详情

4.3 g (20.6 mmol) of N-[2-(4-fluoro-3-methylphenyl)-1,1-dimethylethyl]formamide, 20 mL concentrated hydrochloric acid, and 20 mL water are refluxed for 2 hours. The reaction mixture is diluted with water, made alkaline with concentrated sodium hydroxide solution, and extracted with dichloromethane. The organic phases are dried with sodium sulfate and evaporated down. The residue is dissolved in ethyl acetate, combined with ethereal hydrochloric acid, and cooled. The crystals precipitated are suction filtered and washed with diethyl ether and dried. White solid. Yield: 3.9 g (87%, hydrochloride); melting point 196° C.-198° C.

1. extractionextracted with dichloromethane
2. dry with materialThe organic phases are dried with sodium sulfate
3. customevaporated down
4. dissolutionThe residue is dissolved in ethyl acetate
5. temperaturecooled
6. customThe crystals precipitated
7. filtrationare suction filtered
8. washwashed with diethyl ether
9. customdried