HRID2075968

反应详情

EQUATION

反应方程式

HRID 2075968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of [5-benzyloxy-4-methoxy-2-(5-methyl-[1,2,4]oxadiazol-3-yl)phenyl]phenylmethanone (reference example 14-1) (526 mg) and methylene chloride (22 mL) was added titanium(IV) chloride (0.288 mL) at room temperature. After stirring for 30 minutes, 2 mol/L hydrochloric acid and ethyl acetate were added to the mixture at room temperature. The separated organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: 50%-67% ethyl acetate/hexane, gradient elution) to give the title compound (383 mg).

WORKUP

后处理

  1. dry with materialThe separated organic layer was dried over anhydrous magnesium sulfate
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (eluent: 50%-67% ethyl acetate/hexane, gradient elution)