反应详情

温度

60 °C

In a four neck round bottomed flask, 45 gm (0.165 mole) of 2-Chloro-N-(β-oxo-2,5-Dimethoxy phenethyl)-acetamide prepared according to step (b), 27 g (0.415 mole) sodium azide and 8.3 g (0.049 mole) potassium iodide and 900 ml of acetone is charged. The solution is refluxed at 60° C. for 5 hours. After completion of the reaction the reaction mass cooled and filtered to remove inorganics. Acetone is distilled off under atmospheric pressure. Water is added and the resulting yellow lumps are filtered. (Yield: 91%). The solid is recrystallized from methanol. The following physical properties are measured.

1. additionis charged
2. customAfter completion of the reaction the reaction mass
3. temperaturecooled
4. filtrationfiltered
5. customto remove inorganics
6. distillationAcetone is distilled off under atmospheric pressure
7. additionWater is added
8. filtrationthe resulting yellow lumps are filtered
9. customThe solid is recrystallized from methanol