HRID402746

反应详情

EQUATION

反应方程式

HRID 402746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To a stirred solution of 0.30 g (0.84 mmols) of 5 in 10 mL of anhydrous acetonitrile at 5° C., was added 0.4 mL (4.24 mmols) of CCl4, 0.31 mL (1.78 mmols) of diisopropylethylamine and 10 mg (85□mols) of 4-dimethylaminopyridine in that order. After stirring the mixture for 5 min. at 5° C., 0.34 mL (1.27 mmols) of dibenzyl phosphonate 6 was added drop wise and the mixture stirred for 1 h at 5° C. The reaction was quenched with water, extracted the product with ethyl acetate and organic layers were washed with water and brine. Filtration of the product through a plug of silica gel afforded 0.52 g of the product 7 as brown liquid.

WORKUP

后处理

  1. stirringthe mixture stirred for 1 h at 5° C
  2. customThe reaction was quenched with water
  3. extractionextracted the product with ethyl acetate and organic layers
  4. washwere washed with water and brine
  5. filtrationFiltration of the product through a plug of silica gel