HRID1947646

反应详情

EQUATION

反应方程式

HRID 1947646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Palladium/Carbon (10% wt) (25 mg, 0.13 mmol) was added to a stirred solution of 4,4-dimethyl-7-nitro-3,4-dihydro-2H-isoquinolin-1-one (250 mg, 1.13 mmol) and ammonium formate (350 mg, 5.65 mmol) in anhydrous DMF (10 ml) at room temperature. The resulting suspension was then heated at reflux for 1 hrs, then cooled and filtered through a pad of celite. The solvent was evaporated and the crude residue purified by flash column chromatography (5% methanol in dichloromethane) to afford the title compound as a pale yellow solid (210 mg, 98%). HPLC retention time 1.00 min. Mass spectrum (ES+) m/z 191 (M+H).

WORKUP

后处理

  1. temperatureThe resulting suspension was then heated
  2. temperatureat reflux for 1 hrs
  3. temperaturecooled
  4. filtrationfiltered through a pad of celite
  5. customThe solvent was evaporated
  6. customthe crude residue purified by flash column chromatography (5% methanol in dichloromethane)