HRID446562

反应详情

EQUATION

反应方程式

HRID 446562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound (625 mg, 0.901 mmol) obtained in Example 1j was dissolved in dichloromethane (9 mL), triethylamine (0.376 mL, 2.70 mmol) and isobutyl chloroformate (183 μL, 1.35 mmol) were added under ice cooling, and the mixture was stirred at the same temperature. The compound (467 mg, 2.70 mmol) obtained in Example 68a was added under ice cooling, and then the temperature was increased to room temperature. After the reaction was completed, a saturated aqueous sodium hydrogencarbonate solution was added, and the mixture was extracted with dichloromethane (×2). The resulting organic layer was dried with anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by NH silica gel column chromatography (a elution solvent, ethyl acetate) to give the title compound (615 mg; yield, 79%).

WORKUP

后处理

  1. extractionthe mixture was extracted with dichloromethane (×2)
  2. dry with materialThe resulting organic layer was dried with anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe resulting residue was purified by NH silica gel column chromatography (a elution solvent, ethyl acetate)