HRID1793887

反应详情

EQUATION

反应方程式

HRID 1793887 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dry HCl gas was bubbled through a cooled (−15° C.) solution of 3,5-dimethoxybenzonitrile (1.50 g, 9.20 mmol) for 30 minutes. The reaction mixture was placed in a refrigerator overnight. After evaporation of the solvent, a white solid was obtained which was dissolved in ethanol. 9.2 ml of a 2 molar solution of ammonia in Methanol was added and the reaction mixture was stirred at room temperature overnight. After evaporation of the solvent, the title compound, MS: m/e=181.2 (M+H+), (1.21 g, 71%) was obtained by chromatographic purification of the residue (silica gel, MeOH, DCM). 1H-NMR (300 MHz, d6-DMSO, 25° C.): δ(ppm)=3.80 (6H, s), 6.82 (1H, t, J=2 Hz), 7.05 (2H, t, J=2 Hz), 9.35 (3H, bs).

WORKUP

后处理

  1. customDry HCl gas was bubbled through
  2. customwas placed in a refrigerator overnight
  3. customAfter evaporation of the solvent
  4. customa white solid was obtained which
  5. customAfter evaporation of the solvent