HRID1037771

反应详情

EQUATION

反应方程式

HRID 1037771 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Nitro-isochromen-1-one (1.0 g, 0.0052 mol) and C-(tetrahydro-pyran-4-yl)-methylamine (0.72 g, 0.0063 mol) were stirred in 1,4-dioxane (3 mL, 0.04 mol) at 120° C. for 18 hours. The mixture was diluted with EtOAc (200 mL), washed with 1 N HCl (30 mL×2), brine (30 mL) and dried over Na2SO4. After the filtration the solvent was removed and the residue was purified via flash chromatography (40 g of silica gel, 40% EtOAc/Hexanes) to give a yellow oil. MS m/z (M+H) 289.1.

WORKUP

后处理

  1. washwashed with 1 N HCl (30 mL×2), brine (30 mL)
  2. dry with materialdried over Na2SO4
  3. filtrationAfter the filtration the solvent
  4. customwas removed
  5. customthe residue was purified via flash chromatography (40 g of silica gel, 40% EtOAc/Hexanes)
  6. customto give a yellow oil