HRID1516705

反应详情

EQUATION

反应方程式

HRID 1516705 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 550 mg (1.39 mmol) of 6-formyl-7-isopropyl-2,2-dimethyl-4-oxo-3,4-dihydro-2H-chromen-5-yl trifluoromethanesulfonate (Example 19A), 202 mg (1.81 mmol) of cyclopent-1-en-1-ylboronic acid, 112 mg (100 μmol) of tetrakis(triphenylphosphine)palladium and 503 mg (2.37 mmol) of potassium phosphate in 8 ml of degassed dioxane and stirred at 100° C. overnight. After cooling to room temperature, ammonium chloride solution is added and the mixture is extracted twice with ethyl acetate. The combined organic phases are dried over sodium sulfate, the solvent is then removed under reduced pressure and the residue is purified by column chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 20:1).

WORKUP

后处理

  1. extractionthe mixture is extracted twice with ethyl acetate
  2. dry with materialThe combined organic phases are dried over sodium sulfate
  3. customthe solvent is then removed under reduced pressure
  4. customthe residue is purified by column chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 20:1)