反应详情

Ethyl 2-ethoxy-5-(4-ethyl-1-piperazinylsulfonyl)nicotinoate (10.2 g, 0.0275 mol) was dissolved in toluene (50 mL) and a solution of sodium hydroxide (1.1 g, 0.0275 mol) in water (20 mL) added to it. This two phase mixture was then stirred vigorously at ambient temperature overnight. The aqueous phase was separated off and adjusted to pH=5.6 by addition of conc. hydrochloric acid. The precipitated product was slurried with ice cooling for 15 minutes, filtered, water washed and dried under vacuo at 50° C. to afford the sub-title compound (4.1 g, 43%) as an off-white solid. Mpt 206–207° C. δ (CDCl3): 1.25 (3H, t), 1.39 (3H, t), (2H, q), 3.03 (4H, m), 3.25 (4H, m), 4.50 (2H, q), 8.25 (1H, d), 8.56 (1H, d). m/z (Found:344 [M+H]+, 100%. C14H22N3O5S requires 344.38).

1. customThe aqueous phase was separated off
2. additionadjusted to pH=5.6 by addition of conc. hydrochloric acid
3. waitThe precipitated product was slurried with ice cooling for 15 minutes
4. filtrationfiltered
5. washwater washed
6. customdried under vacuo at 50° C.