HRID1501760

反应详情

EQUATION

反应方程式

HRID 1501760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A mixture of tert-butyl 1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate (1.83 g, 7.20 mmol), commercially available 4-bromofuran-2(5H)-one (1.41 g, 8.63 mmol), Xantphos (0.416 g, 0.720 mmol), water (0.389 mL, 21.6 mmol), and potassium carbonate (1.989 g, 14.39 mmol) in toluene (50 mL) was degassed with nitrogen followed by addition of palladium acetate (0.081 g, 0.36 mmol). The resulting mixture was heated at 65° C. for 16 h. After filtration through CELITE®, the filtrate was concentrated and the residue was purified on silica gel column using EtOAc /hexane as eluting solvents to give the title compound. LC/MS: (M+1)+: 337.18.

WORKUP

后处理

  1. customwas degassed with nitrogen
  2. filtrationAfter filtration through CELITE®
  3. concentrationthe filtrate was concentrated
  4. customthe residue was purified on silica gel column
  5. washas eluting solvents