HRID1464335

反应详情

EQUATION

反应方程式

HRID 1464335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of ethyl 3-oxo-4-nonenate (1.00 g, 5.04 mmol) and N,N-dimethylformamide dimethyl acetal (0.94 ml, 7.08 mmol) in benzene (10 ml) was stirred at 70° C. for 1.5 hours under nitrogen stream. After cooling, a solution of 4-aminomethyl-2'-t-butoxycarbonylbiphenyl (2.86 g, ca. 10.1 mmol) in tetrahydrofuran (15 ml) was added to the reaction solution and the solution was stirred at room temperature for 2 hours and then concentrated to dryness. The resulting residue was purified by column chromatography on silica gel. The column was eluted with dichloromethane-ethyl acetate (1% to 5%) to give 1.65 g (66.6%) of the title compound as an oil.

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationconcentrated to dryness
  3. customThe resulting residue was purified by column chromatography on silica gel
  4. washThe column was eluted with dichloromethane-ethyl acetate (1% to 5%)