反应详情

A solution of 5.66 gm (0.03 mole) of phenyl carbazate hydrochloride, 3.63 gm (0.03 mole) of 4-acetylpyridine and 50 ml of ethanol is refluxed 2 hr. The solution is cooled and evaporated to dryness in vacuo to give an oil. The oil is triturated with ethyl acetate-methanol to afford a solid. The solid is dissolved in 50 ml of water and treated with 50 ml water containing 5 gm sodium carbonate. A gummy solid separates which solidifies on standing. The crude product is collected and crystallized from ethyl acetate-Skellysolve B to yield 4.13 gm (54%) of the title compound having a melting point of 120.4° C. (decomp.).

1. temperatureThe solution is cooled
2. customevaporated to dryness in vacuo
3. customto give an oil
4. customThe oil is triturated with ethyl acetate-methanol
5. customto afford a solid
6. customThe crude product is collected
7. customcrystallized from ethyl acetate-Skellysolve B