反应详情

To the product of Step B (120 mg, 0.52 mmol) was added a solution of 4-(dimethylamino)pyridine (183 mg, 1.5 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (248 mg, 1.3 mmol) in t-butanol (5 mL) and dichloromethane (5 mL). The reaction mixture was stirred for 15 minutes, 2-chloro-5-methoxybenzenesulfonamide (92 mg, 0.41 mmol) was added, and stirring was continued at room temperature overnight. Dichloromethane (100 mL) was then added, the mixture was washed with 1 N hydrochloric acid (3×100 mL), and the combined organic phases were dried over magnesium sulfate and concentrated under reduced pressure to afford a solid. The solid was rinsed with diethyl ether and dried to afford. 89 mg of the title compound, a compound of this invention, as a white solid, m.p. 236-237° C. 1H NMR (CDCl3) δ 9.99 (br s, 1H), 9.23 (s, 1H), 8.56 (s, 1H), 8.32 (s, 1H), 7.86 (s, 1H), 7.37 (d, 1H), 7.10 (dd, 1H) 3.91 (s, 3H).

1. stirringstirring
2. waitwas continued at room temperature overnight
3. washthe mixture was washed with 1 N hydrochloric acid (3×100 mL)
4. dry with materialthe combined organic phases were dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customto afford a solid
7. washThe solid was rinsed with diethyl ether
8. customdried
9. customto afford