HRID1600860

反应详情

EQUATION

反应方程式

HRID 1600860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of ethyl-2,6-difluorobenzene-carboxylate (EXAMPLE 1C; 373 mg, 2.0 mmol) in DMSO (0.5 ml) was added to a solution of the solid prepared above in DMSO (1.0 ml). The brownish solution was heated at 80° C. for 2 hours. The solvent was evaporated, the solid filtered, washed with water several times and dried. The crude product was purified by flash column chromatography on silica gel using 3-15% ethyl acetate in hexane to give 371 mg of the product (61% yield) as a light yellow oil and unreacted sesamol.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. filtrationthe solid filtered
  3. washwashed with water several times
  4. customdried
  5. customThe crude product was purified by flash column chromatography on silica gel using 3-15% ethyl acetate in hexane