HRID2106566
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
One hundred g of 1-phenylsemicarbazide was added to 500 ml of trimethyl orthoformate, and about 400 mg of p-toluenesulfonic acid was added to the mixture. It was heated on a steam bath with strong agitation for 2 hours, and was then transferred to a large flask, cooled and evaporated under vacuum. The residue was recrystallized from about 1600 ml of acetic acid to obtain 97 g of the desired intermediate, m.p. 277°-280°.
WORKUP
后处理
- additionwas added to the mixture
- temperatureIt was heated on a steam bath with strong agitation for 2 hours
- customwas then transferred to a large flask
- temperaturecooled
- customevaporated under vacuum
- customThe residue was recrystallized from about 1600 ml of acetic acid