HRID866383

反应详情

EQUATION

反应方程式

HRID 866383 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl magnesium iodide prepared from magnesium (0.72g.; 0.03 mole) and methyl iodide (1.42g.; 0.01 mole) in ether (20ml) using standard methods, 4-bromo-phenylbenzyl ether in ether (20ml) was added dropwise with stirring then stirred until reaction was complete (1hr.). Ethyl chloroformate (3.24g.; 0.03 mole) in dry ether (20ml) was then added to the reaction mixture which was then boiled under reflux for 2 hrs. After cooling the reaction mixture was allowed to stand at room temperature for two days then worked up by the addition of water (40ml) and dilute hydrochloric acid (20ml). Separation of the ether layer followed by drying (anhyd. MgSO4), yielded 4-ethoxycarbonylphenoxy phenyl methane, m.p. 45° C.

WORKUP

后处理

  1. additionwas added dropwise
  2. stirringthen stirred until reaction
  3. custom(1hr.)
  4. temperatureunder reflux for 2 hrs
  5. temperatureAfter cooling the reaction mixture
  6. customSeparation of the ether layer
  7. dry with materialby drying (anhyd. MgSO4)