HRID1947630

反应详情

EQUATION

反应方程式

HRID 1947630 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) (63 mg, 0.30 mmol) was added to a stirred solution of 2-ethyl-5-nitro-2,3-dihydro-isoindol-1-one (634 mg, 3.06 mmol) and ammonium formate (949 mg, 15.31 mmol) in anhydrous DMF (12 ml) at room temperature. The resulting suspension was heated at reflux for 1 hr, then cooled and filtered through a pad of celite. The solvent was evaporated in vacuo and the crude residue purified by flash column chromatography (5% methanol in dichloromethane) to yield the title compound as a pale yellow oil (530 mg, 98%). HPLC retention time 0.95 min. Mass spectrum (ES+) m/z 177 (M+H).

WORKUP

后处理

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