HRID1532609

反应详情

EQUATION

反应方程式

HRID 1532609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,3-Dichloro-6-nitroaniline (20.11 g, 97.14 mmol), Raney-nickel (4.78 g of a 50% slurry in water), and ethanol (250 mL) were combined in an autoclave which was pressurized to 150 psig with hydrogen. The resulting reaction mixture was allowed to stir at RT overnight. The mixture was then filtered through a pad of celite, which was subsequently washed with several portions of methanol, and the solvents were removed by rotary evaporation to leave a dark brown solid. The solid was slurried and in hexanes and was collected on a Büchner funnel to afford 16.31 g (95%) of a brown solid. MS (EI): m/z 177.0 (M+H).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. filtrationThe mixture was then filtered through a pad of celite, which
  3. washwas subsequently washed with several portions of methanol
  4. customthe solvents were removed by rotary evaporation
  5. customto leave a dark brown solid
  6. customwas collected on a Büchner funnel