反应详情

1 g (0.0285 mol) of N-[2-(4-(2-hydroxyethoxy)-phenyl)-1-methyl-ethyl]-2-hydroxy-2-(6-chloro-pyridin-2-yl)-ethanamine is dissolved in 40 ml of methylene chloride, 0.28 g (0.00285 mol) of triethylamine are added and then 0.322 g (0.00285 mol) of chloroacetyl chloride are added dropwise thereto with stirring in an ice bath. The reaction solution is stirred at ambient temperature for 40 minutes and evaporated down. The residue is dissolved in 10 ml of dimethylformamide, 110 mg (0.00234 mol) of 50-55% sodium hydride in oil are added and the resulting mixture is stirred for 30 minutes at ambient temperature. It is then carefully decomposed with 30 ml of water, acidified with 2N hydrochloric acid and then made alkaline with 2N ammonia. The product is extracted with methylene chloride, dried over sodium sulphate and concentrated by evaporation. The residue is purified over a silica gel column using ethyl acetate as eluant.

1. stirringThe reaction solution is stirred at ambient temperature for 40 minutes
2. customevaporated down
3. dissolutionThe residue is dissolved in 10 ml of dimethylformamide
4. stirringthe resulting mixture is stirred for 30 minutes at ambient temperature
5. extractionThe product is extracted with methylene chloride
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated by evaporation
8. customThe residue is purified over a silica gel column