反应详情

To a mixture of cyanoacetic acid (VII) 2.34 g (27.5 mmol) and benzyl alcohol (VIIIa) 2.70 g (25 mmol) in 60 mL of toluene 50 mg of p-TsOH was added and the mixture was refluxed in a flask with a Dean-Stark trap for 24 h. The mixture was cooled down and toluene was washed with H2O and toluene was evaporated. The residue was distilled in vacuo (Kugelrohr apparatus, 0.1 mm Hg, T. oven 170-180° C.). Yield 3.36 g (77%), a colorless oil. MS (m/z, rel. intensity, %): 167.0 ([M+NH4−CN]+, 27), 193.0 ([M+NH4]+, 100).

1. additionwas added
2. temperaturethe mixture was refluxed in a flask with a Dean-Stark trap for 24 h
3. temperatureThe mixture was cooled down
4. washtoluene was washed with H2O and toluene
5. customwas evaporated
6. distillationThe residue was distilled in vacuo (Kugelrohr apparatus, 0.1 mm Hg, T. oven 170-180° C.)