HRID2233069

反应详情

EQUATION

反应方程式

HRID 2233069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 6-bromo-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene (61.3 mmol) and 4-amino-3-nitrobenzonitrile (61.3 mmol) in THF (150 mL) are added NaOtBu (67.4 mmol), 2-(t-butylphosphino)biphenyl (6.13 mmol), and Pd2(bda)3 (3.06 mmol) at room temperature. The reaction mixture is heated at 80° C. for 2 h. After cooling, the mixture is filtered through Celite. The filtrate is diluted with H2O and extracted with EtOAc. The organic layer is dried over MgSO4 and evaporated in vacuo. The resulting solid is washed with a mixture of hexane and EtOAc (8:1) to give (30).

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe mixture is filtered through Celite
  3. additionThe filtrate is diluted with H2O
  4. extractionextracted with EtOAc
  5. dry with materialThe organic layer is dried over MgSO4
  6. customevaporated in vacuo
  7. washThe resulting solid is washed with a mixture of hexane and EtOAc (8:1)