反应详情

5-(6-Methoxy-pyridin-3-yl)-4-methyl-thiophene-2-sulfonyl chloride (0.19 g, 0.63 mmol) was dissolved in acetone (6 ml) and added dropwise to an aqueous ammonium hydroxide solution (25%, 1.2 ml). After 1 hour the solvent was removed under reduced pressure, the residue diluted with water and extracted with ethyl acetate (3×). The combined organic extracts were washed with water, brine, dried (MgSO4.2H2O), filtered and concentrated under reduced pressure to yield a crude that was purified over silica gel (n-heptane-ethyl acetate 1:2 to 2:1 v/v) to yield a beige solid: 0.12 g (62%), MS: m/e 283.0 (MH−).

1. customAfter 1 hour the solvent was removed under reduced pressure
2. additionthe residue diluted with water
3. extractionextracted with ethyl acetate (3×)
4. washThe combined organic extracts were washed with water, brine
5. dry with materialdried (MgSO4.2H2O)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customto yield a crude that
9. customwas purified over silica gel (n-heptane-ethyl acetate 1:2 to 2:1 v/v)
10. customto yield a beige solid