反应详情

温度

60 °C

2-[6-(Aminomethyl)-2-pyridyl]-4H-1,3-benzothiazine-4-one trifluoroacetic acid salt (350 mg, 0.91 mmol) was dissolved in N,N-dimethylacetamide (10 ml), and 2-thenoyl chloride (400 mg, 2.72 mmol) was added thereto. The reaction mixture was stirred at 60° C. for 15 hrs and combined with ethyl acetate and water. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-ethylacetate (1:4, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (151 mg, 43%) as white crystals.

1. washThe organic layer was washed with saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customThe solvent was evaporated
4. washThe fractions eluted with hexane-ethylacetate (1:4, v/v)
5. customwere collected
6. concentrationconcentrated
7. customrecrystallized from hexane-tetrahydrofuran