HRID1181027

反应详情

EQUATION

反应方程式

HRID 1181027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-(2-benzyloxy-ethyl)-2-(4-bromo-phenyl)-5-methyl-oxazole (0.025 mol, 9.2 g), phenol (0.03 mol, 2.8 g), K3PO4 (0.05 mol, 10.6 g), 2-(di-tert-butylphosphino)biphenyl (1.8 mmol, 0.54 g) and Pd(OAc)2 (1.2 mmol, 0.28 g) in toluene (350 mL) was degassed with nitrogen and heated at 100° C. for 18 h. Additional Pd(OAc)2 (0.5 g) and phosphine ligand (1.0 g) were added, and the mixture was heated 5 h at 100° C. The reaction was concentrated and purified directly by silica gel chromatography (4/1 hexanes/ethyl acetate) to give the title compound (7.6 g).

WORKUP

后处理

  1. customwas degassed with nitrogen
  2. additionAdditional Pd(OAc)2 (0.5 g) and phosphine ligand (1.0 g) were added
  3. temperaturethe mixture was heated 5 h at 100° C
  4. concentrationThe reaction was concentrated
  5. custompurified directly by silica gel chromatography (4/1 hexanes/ethyl acetate)