HRID502732

反应详情

EQUATION

反应方程式

HRID 502732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To an orange solution of 3-(2-nitro-4-(trifluoromethyl)phenyl)pyridine (1.4 g, 5.2 mmol) in 2 ml acetone and 1 mL benzene was added iodomethane (1.0 ml, 16 mmol). The solution was allowed to stand for 5 days, and was concentrated in vacuo to give an orange solid. A portion of this material was treated with platinum (IV) oxide (0.11 g, 0.49 mmol) in 5 ml MeOH under an atmosphere of hydrogen for approximately 24 h. The reaction was flushed with nitrogen, filtered through celite, and concentrated. Purification by silica gel chromatography (MC/MeOH/conc. NH4OH) provided the title compound. MS (m/z): 259.0 (M+H)+. Calc'd for C13H17F3N2: 258.28.

WORKUP

后处理

  1. concentrationwas concentrated in vacuo
  2. customto give an orange solid
  3. customThe reaction was flushed with nitrogen
  4. filtrationfiltered through celite
  5. concentrationconcentrated
  6. customPurification by silica gel chromatography (MC/MeOH/conc. NH4OH)