HRID2358790

反应详情

EQUATION

反应方程式

HRID 2358790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product from Example 193a (1.00 g, 4.9 mmol), and the product from Example 197b (0.90 g, 5.4 mmol) and K2CO3 (0.86 g, 6.2 mmol) in DMF (20 mL) were heated at 100° C. for 10 hours. The reaction mixture was cooled to room temperature, diluted with H2O. The resulting solid was collected by filtration, washed with H2O, and dried in vacuum to give brown crystal, which was purified by silica gel column chromatography eluting with 5:2 EtOAc/hexane to give the title compound as a dark orange crystal (0.47 g, 30%).

WORKUP

后处理

  1. filtrationThe resulting solid was collected by filtration
  2. washwashed with H2O
  3. customdried in vacuum
  4. customto give brown crystal, which
  5. customwas purified by silica gel column chromatography
  6. washeluting with 5:2 EtOAc/hexane