HRID2075971

反应详情

EQUATION

反应方程式

HRID 2075971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of [3-hydroxy-4-methoxy-6-(5-methyl-[1,2,4]oxadiazol-3-yl)-2-nitrophenyl]phenylmethanone (reference example 22-1) (377 mg) and ethyl acetate (10.6 mL) were added aluminum chloride (361 mg) and pyridine (0.387 mL). The mixture was refluxed for 2.5 hours. After cooling to room temperature, 1 mol/L hydrochloric acid was added to the mixture. The separated organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with hexane:methylene chloride=4:1 to give the title compound (317 mg) as an amorphous.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2.5 hours
  2. washThe separated organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was triturated with hexane