HRID1640136

反应详情

EQUATION

反应方程式

HRID 1640136 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a solution of 2-[3-(2,5-dimethyl-1H-pyrrol-1-yl)-5-(trifluoromethyl)phenyl]-propan-2-ol (2.29 g, 7.70 mmol) in EtOH (70 mL) and water (41 mL), was added hydroxylamine hydrochloride (16.1 g, 23.1 mmol) and potassium hydroxide (8.64 g, 154 mmol). The reaction mixture was heated at 110° C. for 18 h, and then allowed to cool to rt. The solvents were evaporated and the residue was dissolved in water and extracted with EtOAc (2×). The organic solutions were combined, washed with brine, dried over Na2SO4, filtered and evaporated. The residue was triturated with Et2O and the filtrate was evaporated to provide -[3-amino-5-(trifluoromethyl)phenyl]propan-2-ol (1.70 g, quant). 1H NMR (400 MHz,CDCl3) δ: 7.08 (s, 1H), 6.99 (s, 1H), 6.79 (s, 1H), and 1.56 (s, 6H).

WORKUP

后处理

  1. temperatureto cool to rt
  2. customThe solvents were evaporated
  3. dissolutionthe residue was dissolved in water
  4. extractionextracted with EtOAc (2×)
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was triturated with Et2O
  10. customthe filtrate was evaporated