反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of the compound of Example 223 (20 mg, 0.0388 mmol) in THF (10 ml) was added aqueous solution of lithium hydroxide (4 mg, 0.0776 mmol, 2 eq) and the mixture was stirred at RT for 2 h. The mixture was quenched and extracted as in Example 1(d). The solvent was distilled off to afford the crude residue which was purified by preparative HPLC to give the pure product in 90% yield (25 mg). 1H NMR (400 MHz, DMSO-d6): δ 10.7 (s, 1H), 8.77 (s, 1H), 8.23 (s, 1H), 8.10 (s, 1H), 8.01 (s, 1H), 7.97 (s, 1H), 7.83 (s, 1H), 7.78 (d, 1H), 7.73 (d, 1H), 7.65 (d, 1H), 7.59 (s, 1H), 7.49 (t, 1H), 7.3 (t, 1H), 3.90 (s, 3H), 3.45 (s, 2H); LC-MS (ESI): Calculated mass: 487.15; Observed mass: 488.0 [M+H]+ (rt: 0.638 min).
WORKUP
后处理
- customThe mixture was quenched
- extractionextracted as in Example 1(d)
- distillationThe solvent was distilled off