HRID1909457

反应详情

EQUATION

反应方程式

HRID 1909457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[3-(4-Cyclopropyl-4H-[1,2,4]triazol-3-yl)-phenyl]-carbamic acid benzyl ester (60 mg, 0.17 mmol) was dissolved in HBr solution (1 mL, 33% in acetic acid) and the reaction mixture was stirred overnight. The solvent was removed and the residue was neutralized with saturated sodium bicarbonate solution before being poured into brine. The aqueous phase was extracted 5 times with ethyl acetate. The organic phase was dried with sodium sulfate and the solvent was removed to obtain 3-(4-cyclopropyl-4H-[1,2,4]triazol-3-yl)-phenylamine as an off-white powder (30 mg, 88%). 201.1 (M+1). 1H NMR of HBr salt (DMSO) d 9.24 (s, 1H), 7.50-7.63 (m, 3H), 6.6-8.0 (br, 4H I H2O), 3.65 ppm (m, 1H), 1.05 (m, 4H).

WORKUP

后处理

  1. customThe solvent was removed
  2. additionbefore being poured into brine
  3. extractionThe aqueous phase was extracted 5 times with ethyl acetate
  4. dry with materialThe organic phase was dried with sodium sulfate
  5. customthe solvent was removed