HRID2248301

反应详情

EQUATION

反应方程式

HRID 2248301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6,7-dichloro-4H-1-benzopyran-4-carboxylic acid (16.8 gm), tetra (N-butyl)ammonium hydrogensulfate (23 gm), benzyl bromide (9.7 mL), saturated sodium bicarbonate (100 mL) and dichloromethane (100 mL) were stirred vigorously at room temperature for 14 hours, then diluted with dichloromethane, and the organic layer separated, washed with saturated sodium bicarbonate, water, brine, dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (2:1 dichloromethane/hexanes, SiO2) to afford the title compound (11.8 gm, Rf=0.3 (2:1 dichloromethane/hexanes, SiO2).

WORKUP

后处理

  1. customthe organic layer separated
  2. washwashed with saturated sodium bicarbonate, water, brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by column chromatography (2:1 dichloromethane/hexanes, SiO2)