HRID1868078

反应详情

EQUATION

反应方程式

HRID 1868078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred solution of tert-butyl-4-(4-fluoro-2-(trifluoromethyl)phenyl)piperazine-1-carboxylate (6.8 g, 19.5 mmol) in anhydrous dichloromethane (90 mL) was added TFA (45 mL) dropwise at 0° C. The reaction mixture was stirred at 0° C. for 15 minutes then the cooling bath was removed and it was allowed to stir at room temperature for 2 hours. Reaction was complete as determined by TLC. Most of TFA was azeotropped with dichloroethane. The residue was then diluted with dichloromethane and washed with saturated Na2CO3 (aq.). Organic layer was dried over MgSO4. Solvent evaporation afforded 1-(4-fluoro-2-(trifluoromethyl)phenyl)piperazine in 79.9% yield (3.86 g) as light brown oil. 1H NMR (400 MHz, CHLOROFORM-D) δ ppm 2.78-2.90 (m, 4H) 2.96-3.04 (m, 4H) 7.18-7.25 (m, 1H) 7.29-7.42 (m, 2H).

WORKUP

后处理

  1. customthe cooling bath was removed
  2. stirringto stir at room temperature for 2 hours
  3. customReaction
  4. washwashed with saturated Na2CO3 (aq.)
  5. dry with materialOrganic layer was dried over MgSO4
  6. customSolvent evaporation