反应详情

Sodium pellets (9.8 g, 0.43 mol) were added portionwise to a solution of 2,4-dimethylphenylacetonitrile (48 g, 0.33 mol) in ethyl acetate (150 mL) at ambient temperature. The reaction mixture was heated to reflux temperature and stirred for 16 hours. The resulting suspension was cooled to room temperature and filtered. The collected precipitate was washed with copious amounts of ether and then air-dried. The solid was dissolved in water and a 1N HCl solution was added until the pH=5-6. The mixture was extracted with ethyl acetate (3×200 mL); the combined organic layers were dried over MgSO4 and filtered. Solvent was removed in vacuo to afford a white solid (45.7 g, 74% yield): NMR (CDCl3, 300 MHz) :; CI-MS: 188 (M+H).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux temperature
3. filtrationfiltered
4. washThe collected precipitate was washed with copious amounts of ether
5. customair-dried
6. dissolutionThe solid was dissolved in water
7. additiona 1N HCl solution was added until the pH=5-6
8. extractionThe mixture was extracted with ethyl acetate (3×200 mL)
9. dry with materialthe combined organic layers were dried over MgSO4
10. filtrationfiltered
11. customSolvent was removed in vacuo