反应详情

2 g (13.2 mmol) of 4-(2-methoxy-ethyl)-phenylamine (Example 42b) and 1.85 g (13.9 mmol) of N-chlorosuccinimide (Aldrich, Buchs, Switzerland) in 26 ml of isopropanol are stirred at rt for 30 min. The reaction mixture is evaporated to dryness and the residue is taken in EtOAc. The organic layers is washed with sat. aqueous NaHCO3 (2×), dried over MgSO4, filtered and evaporated. The residue is purified by flash chromatography on silica gel (hexane-EtOAc 5:1 to 2:1) to provide the title compound as an oil. ES-MS: 186 (M+H)+; analytical HPLC: tret=2.42 minutes (Grad 1).

1. customThe reaction mixture is evaporated to dryness
2. washThe organic layers is washed with sat. aqueous NaHCO3 (2×)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated
6. customThe residue is purified by flash chromatography on silica gel (hexane-EtOAc 5:1 to 2:1)