HRID1700522

反应详情

EQUATION

反应方程式

HRID 1700522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 3-carboxy-4-oxo-6-phenyl-4,5,6,7-tetrahydrobenzofuran (1.28 g) in dichloromethane (25 ml) were added, under ice-cooling, WSC (1.15 g) and N-hydroxybenzotriazole (0.92 g), and the mixture was stirred at room temperature for 30 minutes. To the mixture was added concentrated ammonia solution (4.1 g), and the mixture was stirred at room temperature overnight (12 hours). To the reaction solution was added water, and the mixture was subjected to extraction. The lower layer was washed with saturated brine, dried (anhydrous magnesium sulfate) and concentrated under reduced pressure, and the residue was washed with ethyl acetate and isopropylether to give 3-carbamoyl-6-phenyl-4,5,6,7-tetrahydrobenzofuran-4-one (0.36 g).

WORKUP

后处理

  1. additionwere added, under ice-
  2. temperaturecooling
  3. extractionthe mixture was subjected to extraction
  4. washThe lower layer was washed with saturated brine
  5. dry with materialdried (anhydrous magnesium sulfate)
  6. concentrationconcentrated under reduced pressure
  7. washthe residue was washed with ethyl acetate and isopropylether