HRID2106566

反应详情

EQUATION

反应方程式

HRID 2106566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added to the mixture
  2. temperatureIt was heated on a steam bath with strong agitation for 2 hours
  3. customwas then transferred to a large flask
  4. temperaturecooled
  5. customevaporated under vacuum
  6. customThe residue was recrystallized from about 1600 ml of acetic acid