HRID474723

反应详情

EQUATION

反应方程式

HRID 474723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

{2-[4-(4-Chloro-phenoxy)-phenyl]ethyl}-carbamic acid tert-butyl ester (600 mg, 1.72 mmol, 1 eq) and TFA (658 μl) were dissolved in 50 ml of dry DCM under argon atmosphere. The mixture was stirred at room temperature for 60 hours. The solvent was evaporated, the resulting crude was dissolved in 10 ml of MeOH and was purified using 20 g SCX column. The free base was rinsed from the column using 1N NH3/ethanol solution. The solvent was evaporated and obtained was 2-[4-(4-chloro-phenoxy)-phenyl]-ethylamine (404 mg, yield=90.8%, purity=96%) in form of yellowish oil. MS: [M+H]+=248.21 1H NMR (300 MHz; CDCl3) 8/ppm 1.22 (s, 2H), 2.71 (t, J=6.62 Hz, 2H), 2.95 (t, J=6.62 Hz, 2H), 6.85-6.96 (m, 4H), 7.16 (d, J=7.60 Hz, 2H), 7.25 (d, J=7.60 Hz, 2H)

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe resulting crude was dissolved in 10 ml of MeOH
  3. customwas purified
  4. washThe free base was rinsed from the column
  5. customThe solvent was evaporated
  6. customobtained