HRID1871653

反应详情

EQUATION

反应方程式

HRID 1871653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

0.48 g of sodium hydride (55% oil suspension) was added to a mixture of 2.78 g of diethyl 2-(3-phenylpropyl)malonate, 20 ml of toluene and 10 ml of N,N-dimethylacetamide, and the resulting mixture was stirred at room temperature for 30 minutes. Then, 2.45 g of 4-benzyloxybenzyl chloride was added to the reaction mixture, and the mixture was stirred at room temperature for 30 minutes and then at 60° C. for 30 minutes. After the reaction, ethyl acetate and water were added to the reaction mixture, and then the ethyl acetate layer was separated. The extract thus obtained was dried over anhydrous magnesium sulfate and concentrated. The residue thus obtained was subjected to silica gel column chromatography (ethyl acetate:hexane=1:9) to obtain 3.91 g of the desired compound as a syrup.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. waitat 60° C. for 30 minutes
  3. additionwere added to the reaction mixture
  4. customthe ethyl acetate layer was separated
  5. extractionThe extract thus
  6. customobtained
  7. dry with materialwas dried over anhydrous magnesium sulfate
  8. concentrationconcentrated
  9. customThe residue thus obtained