HRID468276

反应详情

EQUATION

反应方程式

HRID 468276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (7-chlorobenzo[d][1,3]-dioxol-5-yl)methanol (5.5 g, 30 mmol) and SOCl2 (5.0 mL, 67 mmol) in dichloromethane (20 mL) was stirred at room temperature for 1 h and was then poured into ice water. The organic layer was separated and the aqueous phase was extracted with dichloromethane (50 mL×3). The combined extracts were washed with water and aqueous NaHCO3 solution, dried over Na2SO4 and evaporated under reduced pressure to afford 4-chloro-6-(chloromethyl)benzo[d][1,3]dioxole, which was directly used in the next step.

WORKUP

后处理

  1. customThe organic layer was separated
  2. extractionthe aqueous phase was extracted with dichloromethane (50 mL×3)
  3. washThe combined extracts were washed with water and aqueous NaHCO3 solution
  4. dry with materialdried over Na2SO4
  5. customevaporated under reduced pressure