反应详情

A mixture of 3-bromopyridine-2-thiol (0.04 g, 0.2 mmol), 1-bromo-3-chloropropane in DMF (0.424 mmol/mL, 2.0 mL), and K2CO3 (60 mg, 0.424 mmol) in DMF (2.0 mL) was stirred at rt for 10 minutes. The reaction mixture was then concentrated to dryness and the resultant residue diluted with water (10 mL) and extracted with ethyl acetate (3×10 mL). The combined organic extracts were dried over Na2SO4 and concentrated to dryness to give the title compound (0.05 g, 89% purity). MS (ESI): mass calcd. for C8H9BrClNS, 264.93; m/z found, 265.8 [M+H]+.

1. concentrationThe reaction mixture was then concentrated to dryness
2. additionthe resultant residue diluted with water (10 mL)
3. extractionextracted with ethyl acetate (3×10 mL)
4. dry with materialThe combined organic extracts were dried over Na2SO4
5. concentrationconcentrated to dryness