HRID746271

反应详情

EQUATION

反应方程式

HRID 746271 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.54 g (0.005 mole) of 4-(3,5-dichloro-4-methylphenyl)-2-methylthio-4-oxobutyric acid, prepared as described in step (c) above, were suspended in 5 ml of ethanol and then 0.25 g of hydrazine monohydrate was added, at room temperature, to the suspension, after which the mixture was stirred for 1 hour at room temperature. The mixture was then heated under reflux for 6 hours, after which it was cooled and the resulting crystals were collected by filtration and washed with a small amount of ethanol, to give 1.32 g (yield 87.1%) of the desired Compound No. 22, melting at 163°-165° C.

WORKUP

后处理

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux for 6 hours
  3. temperatureafter which it was cooled
  4. filtrationthe resulting crystals were collected by filtration
  5. washwashed with a small amount of ethanol