HRID657340

反应详情

EQUATION

反应方程式

HRID 657340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-bromo-3-(bromomethyl)-5-methylbenzene (40.0 g, 151 mmol), 1,4-dioxane (150 mL), water (150 mL) and calcium carbonate (37.9 g, 379 mmol) was heated for 16 h at reflux. The mixture was filtered and the filtrate was concentrated in vacuum, then diluted with CH2Cl2 (150 mL). The organic layer was washed with HCl (2N, 50 mL) and a solution of saturated sodium bicarbonate (50 mL), dried over (Na2SO4) and concentrated in vacuum to give 25.0 g of crude product (3-bromo-5-methylphenyl)methanol.

WORKUP

后处理

  1. temperaturewas heated for 16 h
  2. temperatureat reflux
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated in vacuum
  5. additiondiluted with CH2Cl2 (150 mL)
  6. washThe organic layer was washed with HCl (2N, 50 mL)
  7. dry with materiala solution of saturated sodium bicarbonate (50 mL), dried over (Na2SO4)
  8. concentrationconcentrated in vacuum