HRID1579205

反应详情

EQUATION

反应方程式

HRID 1579205 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred mixture of 4-chloro-3-trifluoromethylcinnamic acid (50 g, 0.2 mole) in 200 ml of SOCl2 was heated at reflux for 2 hours. The excess SOCl2 was removed in vacuo and the residue flushed with dry benzene. The residue was treated with a mixture of 1-aminohydantoin hydrochloride (30 g, 0.2 mole) in 400 ml of pyridine. The reaction mixture was heated at reflux for 3 hours; then poured into ice/HCl. The crude residue (74 g, 100%) was recrystallized from CH3NO2 (Darco) to give an analytical sample melting at 270°-273°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. customThe excess SOCl2 was removed in vacuo
  4. customthe residue flushed with dry benzene
  5. temperatureThe reaction mixture was heated
  6. temperatureat reflux for 3 hours
  7. customThe crude residue (74 g, 100%) was recrystallized from CH3NO2 (Darco)
  8. customto give an analytical sample melting at 270°-273°