HRID402754

反应详情

EQUATION

反应方程式

HRID 402754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of cesium carbonate (4.27 g, 13.11 mmol), copper (I) iodide (0.832 g, 4.37 mmol), tert-butyl 2-oxo-1-oxa-3,8-diazaspiro[4.5]decane-8-carboxylate (1.12 g, 4.37 mmol), N,N′-dimethylethane-1,2-diamine (0.385 g, 437 mmol) and methyl 4-bromobenzoate (1.128 g, 5.24 mmol) was heated under nitrogen for 18 hours. The crude mixture was filtered through celite. Upon removal of the volatiles, the crude was purified by flash chromatography (EtOAc/hexanes 20 to 100%) to afford the title intermediate as a white solid.

WORKUP

后处理

  1. temperaturewas heated under nitrogen for 18 hours
  2. filtrationThe crude mixture was filtered through celite
  3. customUpon removal of the volatiles
  4. customthe crude was purified by flash chromatography (EtOAc/hexanes 20 to 100%)