反应详情

Methyl 6-(2(benzo[d]isothiazol-3-ylamino)ethylcarbamoyl)nicotinate (211 mg, 0.6 mmol) was dissolved in a mixture of tetrahydrofuran (5 mL) and water (0.5 mL) and treated with lithium hydroxide monohydrate (100 mg, 2.4 mmol). The reaction mixture was stirred at room temperature overnight. The tetrahydrofuran was removed under vacuum and the residue was diluted with water. Dropwise addition of 50% aqueous hydrochloric acid gave a white solid, which was collected by vacuum filtration and dried to yield 6-(2-(benzo[d]isothiazol-3-ylamino)ethylcarbamoyl)nicotinic acid (130 mg) as a white solid. 1H NMR (300 MHz, CDCl3/DMSO-d6): 9.02 (m, 1H), 8.83 (broad s, 1H), 8.32 (m, 1H), 8.10 (d, 1H), 7.95 (d, 1H), 7.68 (d, 1H), 7.39 (t, 1H), 7.25 (t, 1H), 3.71 ppm (m, 4H). MW=342 confirmed by LC-MS, tr=10.56 min (Method Y) MH+=343

1. customThe tetrahydrofuran was removed under vacuum
2. additionthe residue was diluted with water
3. additionDropwise addition of 50% aqueous hydrochloric acid
4. customgave a white solid, which
5. filtrationwas collected by vacuum filtration
6. customdried