HRID2278298

反应详情

EQUATION

反应方程式

HRID 2278298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-iodo-1-(methyloxy)-3-{[(methyloxy)methyl]oxy}benzene (Intermediate 2, 16.2 g, 55.1 mmol) in dichloromethane (100 ml, SCRC) was bubbled HCl (g) for 30 mins. TLC showed that the reaction was completed. The reaction mixture was poured into an aqueous saturated solution of NaHCO3 (200 ml) and extracted with dichloromethane (3×200 ml, SCRC). The combined organic layers were dried, evaporated and purified by column chromatography on silica gel (EtOAc: PE=1:50) to afford the title compound as a yellow liquid (10.3 g).

WORKUP

后处理

  1. extractionextracted with dichloromethane (3×200 ml, SCRC)
  2. customThe combined organic layers were dried
  3. customevaporated
  4. custompurified by column chromatography on silica gel (EtOAc: PE=1:50)