反应详情

The product of Step A was dissolved in tetrahydrofuran (10 mL) and a solution of lithium hydroxide monohydrate (97 mg, 8.3 mmol) in water (5 mL) was added. The reaction mixture was stirred at room temperature for one hour, after which time the tetrahydrofuran was removed on a rotary evaporator under reduced pressure, and water was added (5 mL), followed by the addition of 1 N HCl (5 mL). The resulting suspension was filtered through a glass-fritted filter funnel, and the isolated solid was washed with water and dried over nitrogen to afford 451 mg of the title compound as a solid. 1H NMR ((CD3)2SO) δ 9.33 (s, 1H), 9.30 (s, 1H), 8.69 (s, 1H).

1. customafter which time the tetrahydrofuran was removed on a rotary evaporator under reduced pressure, and water
2. additionwas added (5 mL)
3. additionfollowed by the addition of 1 N HCl (5 mL)
4. filtrationThe resulting suspension was filtered through a glass-fritted filter funnel
5. washthe isolated solid was washed with water
6. customdried over nitrogen