反应详情

Ethyl 2-chloroacetate (10.6 ml, 0.1 mol) is slowly added to hot (105° C.) pyridine (8.9 ml, 0.11 mmol whereby the temperature is maintained in the range of 100° C. to 110° C. The resulting brown oil is dissolve in ethanol (60 ml), β-dimethylamino propiophenone hydrochloride (17.7 g, 0.1 mol; prepared to according to Example 1) and ammonium acetate (60 g) are added and the mixture is boiled under reflux for 4 h. After cooling, the mixture is filtered and the solvent is evaporated in vacuo. The residue is crystallized from water, collected by filtration and purified by re-crystallization from toluene. The title compound is obtained as colorless crystals (4.7 g, 28% of th.) with mp 200° C.

1. temperatureis maintained in the range of 100° C. to 110° C
2. temperatureunder reflux for 4 h
3. temperatureAfter cooling
4. filtrationthe mixture is filtered
5. customthe solvent is evaporated in vacuo
6. customThe residue is crystallized from water
7. filtrationcollected by filtration
8. custompurified by re-crystallization from toluene