HRID406042

反应详情

EQUATION

反应方程式

HRID 406042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Ammonium formate (7.25 g) was added to a suspension of 2-(cis-3-methoxy-cyclohexyloxy)-3-nitro-pyridine (5.80 g) and 10% palladium on charcoal (400 mg) in methanol (40 ml) at room temperature and the mixture was heated to reflux for 30 min until LCMS indicated complete conversion of the starting material. The mixture was diluted with dichloromethane (100 ml) and water (40 ml), filtered through celite, and the filtercake was washed with dichloromethane (30 ml). The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was submitted to column chromatography (silica gel, petrol ether/ethyl acetate 70:30) to give the desired product.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 30 min until LCMS
  3. filtrationfiltered through celite
  4. washthe filtercake was washed with dichloromethane (30 ml)
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo