HRID571067

反应详情

EQUATION

反应方程式

HRID 571067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

To a suspension of 6.6 g (30.5 mmol) 5-(benzyloxy)-2-methyl-4H-pyran-4-one in 150 ml 30% AcOH was added 7.5 g (45.8 mmol) m-aminobiphenyl. The reaction mixture was heated at 160° C. for 18 h, then cooled to rt, extracted with 300 ml EtOAc, washed with brine, and concentrated in vacuo. Purification by flash chromatography (330 g silica gel, 0-20% MeOH:EtOAc) afforded 5-(benzyloxy)-1-biphenyl-3-yl-2-methylpyridin-4(1H)-one. LCMS (M+H)+=368.3.

WORKUP

后处理

  1. temperaturecooled to rt
  2. extractionextracted with 300 ml EtOAc
  3. washwashed with brine
  4. concentrationconcentrated in vacuo
  5. customPurification by flash chromatography (330 g silica gel, 0-20% MeOH:EtOAc)