HRID477894

反应详情

EQUATION

反应方程式

HRID 477894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 12.1 grams (0.0703 mole) of 4chlorophenylthiocarboxamide, 12.1 grams (0.0714 mole) of bromoacetaldehyde dimethyl acetal, and 2 ml of concentrated hydrochloric acid in 280 ml of ethanol was heated at reflux for approximately 18 hours. An additional 1 ml of concentrated hydrochloric acid was added, and the mixture was heated at reflux for two days. The reaction mixture was cooled, and the solvent was removed by evaporation under reduced pressure leaving a residue. This residue was purified by column chromatography on silica gel, eluting with methylene chloride:n-hexane (3:1), to yield 4.8 grams of 2-(4-chlorophenyl)thiazole as a solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for approximately 18 hours
  3. temperaturethe mixture was heated
  4. temperatureat reflux for two days
  5. temperatureThe reaction mixture was cooled
  6. customthe solvent was removed by evaporation under reduced pressure
  7. customleaving a residue
  8. customThis residue was purified by column chromatography on silica gel
  9. washeluting with methylene chloride:n-hexane (3:1)