HRID1750727

反应详情

EQUATION

反应方程式

HRID 1750727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of ethyl 4-piperazin-1-ylbenzoate (1.36 g) and 3,3-diphenylacrylaldehyde (1.56 g) in dichloromethane (10 mL) and methanol (10 mL) was treated with polymer-supported cyanoborohydride (2.47 mmol/g, 6 g), shaken at room temperature for 24 hours, and filtered. The resin was washed with 1:1 dichloromethane/methanol (10 mL×3) and the combined filtrates were concentrated. The concentrate was purified by silica gel chromatography eluting with a gradient from 10%-50% ethyl acetate/hexanes to provide the desired product.

WORKUP

后处理

  1. filtrationfiltered
  2. washThe resin was washed with 1:1 dichloromethane/methanol (10 mL×3)
  3. concentrationthe combined filtrates were concentrated
  4. customThe concentrate was purified by silica gel chromatography
  5. washeluting with a gradient from 10%-50% ethyl acetate/hexanes