反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto cool to rt
- customThe solvents were evaporated
- dissolutionthe residue was dissolved in water
- extractionextracted with EtOAc (2×)
- washwashed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
- customThe residue was triturated with Et2O
- customthe filtrate was evaporated