HRID2361285

反应详情

EQUATION

反应方程式

HRID 2361285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of methyl 2-(bromomethyl)-5-fluorobenzoate (0.750 g, 3.04 mmol) and calcium carbonate (1.823 g, 18.21 mmol) in 1,4-dioxane (30 mL) and water (30.0 mL) was heated at reflux for 2.5 hr. The insoluble material was removed by filtration. The filtrate was concentrated under vacuum and then extracted with CH2Cl2 (4×30 mL). The combined extract was dried over anhydrous MgSO4. Removal of solvent under vacuum provided the desired product (0.423 g, 2.78 mmol, 92% yield) as a white solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hr
  3. customThe insoluble material was removed by filtration
  4. concentrationThe filtrate was concentrated under vacuum
  5. extractionextracted with CH2Cl2 (4×30 mL)
  6. extractionThe combined extract
  7. dry with materialwas dried over anhydrous MgSO4
  8. customRemoval of solvent under vacuum