反应详情

A solution of 1.753 g (7.711 mmol) of N-tert-butoxycarbonyl-2-(3-thienyl)ethylamine, 0.46 g (15.4 mmol) of powdered paraformaldehyde and 73 mg (0.39 mmol) of p-toluenesulfonic acid monohydrate in 150 ml of toluene was refluxed under dehydrating conditions for 0.5 hours in a Dean-Stark trap. The reaction mixture was cooled to room temperature and diluted with ethyl acetate, after which it was washed with aqueous sodium hydrogen carbonate; the organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=15/1 to 9/1) to yield the desired product.

1. washafter which it was washed with aqueous sodium hydrogen carbonate
2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
3. distillationthe solvent was distilled off under reduced pressure
4. customThe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=15/1 to 9/1)