HRID1042682

反应详情

EQUATION

反应方程式

HRID 1042682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To N,N-dimethyl-1-(2-nitro-4-(trifluoromethyl)phenyl)piperidin-4-amine (3.4 g, 11 mmol) was added Pd/C (10%, 0.57 g) under nitrogen. Methanol (25 mL) was added via syringe, and H2 gas was introduced and the mixture stirred vigorously under an atmosphere of H2. After 96 h, the mixture was flushed with nitrogen, filtered through celite and concentrated. The residue was resubjected to the reaction conditions. After 12 h, the reaction was flushed with nitrogen, filtered through celite and concentrated. The resulting solid was triturated with methanol ten times to give the title compound as a pink solid. MS (m/z): 288.2 (M+H)+. Calc'd for C14H20F3N3: 287.32.

WORKUP

后处理

  1. additionH2 gas was introduced
  2. customthe mixture was flushed with nitrogen
  3. filtrationfiltered through celite
  4. concentrationconcentrated
  5. customThe residue was resubjected to the reaction conditions
  6. waitAfter 12 h
  7. customthe reaction was flushed with nitrogen
  8. filtrationfiltered through celite and
  9. concentrationconcentrated
  10. customThe resulting solid was triturated with methanol ten times