反应详情

Potassium carbonate (8.0 g) was added to a solution of 2,2-dimethoxyethylamine in water (90 ml) and acetone (40 ml) at rt. The reaction mixture was cooled in an ice-water bath and 4-bromobenzoyl chloride (16.4 g) dissolved in acetone (70 ml) was added drop-wise over 90 min. The stirred reaction mixture was allowed to warm to rt. After a further 2 h the reaction mixture was extracted into EtOAc (3×75 ml), the combined organics were washed with saturated aqueous sodium hydrogen carbonate, dried (MgSO4) and evaporated to give the amide as an off white solid (18.5 g). LCMS electrospray (+ve) 289 (MH+).

1. temperatureThe reaction mixture was cooled in an ice-water bath
2. additionwas added drop-wise over 90 min
3. customThe stirred reaction mixture
4. extractionAfter a further 2 h the reaction mixture was extracted into EtOAc (3×75 ml)
5. washthe combined organics were washed with saturated aqueous sodium hydrogen carbonate
6. dry with materialdried (MgSO4)
7. customevaporated