反应详情

[2-(4-fluoro-benzyl)-phenyl]-acetonitrile is suspended in acetic acid (0.5 L/mol), water (0.3 L/mol) and sulphuric acid (0.35 L/mol). After 5 hours at reflux, the mixture is cooled down, water (1.2 L/mol) and dichloromethane (0.3 L/mol) are added. The organic extract is washed with water (1.3 L/mol) and sodium hydroxide 50% (0.15 L/mol). After stirring for 20 min., the aqueous layer is separated and washed with CH2Cl2 (0.1 L/mol) which is discarded. The aqueous layer is acidified with concentrated hydrochloric acid (2 eq.). The mixture is stirred during 3 hours, the precipitate is then filtered off and washed with water (0.1 L/mol). Yield: 74%.

1. temperatureAfter 5 hours at reflux
2. temperaturethe mixture is cooled down
3. extractionThe organic extract
4. washis washed with water (1.3 L/mol) and sodium hydroxide 50% (0.15 L/mol)
5. customthe aqueous layer is separated
6. washwashed with CH2Cl2 (0.1 L/mol) which
7. stirringThe mixture is stirred during 3 hours
8. filtrationthe precipitate is then filtered off
9. washwashed with water (0.1 L/mol)