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
CONDITIONS
反应条件
- 温度
- 105 °C
PROCEDURE
实验过程
Aluminum chloride (267g) was added in portions over 30 minutes to a stirred solution of 4-ethylphenol (122.1g.) and 4-chloro-benzoyl chloride (140ml.) in dry 1,1,2,2-tetrachloroethane (800ml.). The mixture was heated at 105°C. for 22 hours with stirring, and on cooling a mixture of ice (600g) and concentrated hydrochloric acid was added slowly, A vigorous reaction occurred and some material was lost. The remaining material was separated and the aqueous fraction extracted twice with chloroform (200ml.), and the combined organic layers evaporated to a dark oil which was distilled in vacuo giving two main fractions: B (17.4g) 150°-160°C at 0.3mmHg; C (110.8g) 160°-168°C at 0.3mmHg. Both remained liquid on cooling.
WORKUP
后处理
- temperatureon cooling
- additionwas added slowly
- customA vigorous reaction
- customThe remaining material was separated
- extractionthe aqueous fraction extracted twice with chloroform (200ml.)
- customthe combined organic layers evaporated to a dark oil which
- distillationwas distilled in vacuo
- customgiving two main fractions
- customB (17.4g) 150°-160°C
- temperatureBoth remained liquid on cooling