HRID2399680

反应详情

EQUATION

反应方程式

HRID 2399680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-(3-nitrophenyl)tetrazole (22 g, 0.12 mol) in ethanol (500 mg) was added 10% palladium on carbon (1.5 g, 7% (w/w)) in hydrochloric acid (23 mg of a 5M solution). The mixture was hydrogenated at 40 psi for 10 min, then the catalyst filtered off and washed with water. The solvents were evaporated in vacuo and the brown solid azeotroped with toluene (4×100 mg). The resulting solid was triturated with hot ethanol to give 5-(3-aminophenyl)tetrazole hydrochloride (16.3 g, 71%) as a beige powder, mp 203°-205° C. 1H NMR (360 MHz, D2O) δ 7.63 (1H, d, J=9 Hz), 7.75 (1H, t, J=8 Hz), 8.00 (2H, m).

WORKUP

后处理

  1. filtrationthe catalyst filtered off
  2. washwashed with water
  3. customThe solvents were evaporated in vacuo
  4. customthe brown solid azeotroped with toluene (4×100 mg)
  5. customThe resulting solid was triturated with hot ethanol