反应详情

温度

40 °C

A mixture of 1 g (3.84 mmol) of 6-chloro-N-cyclopentylpyridine-3-sulfonamide, 1.32 g (9.59 mmol) of K2CO3 and 0.88 mL (4.99 mmol) of [(3-bromopropoxy)methyl]benzene in 8 mL of anhydrous DMF is heated for 12 hours at 40° C. After cooling to room temperature, the medium is taken up in 300 mL of EtOAc, washed successively with water (2×100 mL), saturated NaHCO3 solution (100 mL) and brine (100 mL), dried over Na2SO4 and then concentrated under reduced pressure and purified by chromatography on a column of silica gel, eluting with a cyclohexane/EtOAc gradient of 0 to 10% EtOAc. 1.65 g of N-[3-(benzyloxy)propyl]-6-chloro-N-cyclopentylpyridine-3-sulfonamide are thus obtained in the form of an oil.

1. temperatureAfter cooling to room temperature
2. washwashed successively with water (2×100 mL), saturated NaHCO3 solution (100 mL) and brine (100 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. custompurified by chromatography on a column of silica gel
6. washeluting with a cyclohexane/EtOAc gradient of 0 to 10% EtOAc