HRID520300
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
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A mixture of 123b (1.6 g, 2.6 mmol) in HCl/dioxane (4M, 10 mL) was stirred at 25° C. for 1 h. The mixture was evaporated in vacuo and the residue was purified by reverse-phase prep-HPLC to afford 123d (580 mg, 50%) as a pale yellow solid. MS-ESI: [M+H]+ 450.1. 1H NMR (500 MHz, DMSO-d6) δ 8.53-8.52 (m, 2H), 7.90 (d, J=1.0 Hz, 1H), 7.79-7.76 (m, 1H), 7.45 (d, J=5.0 Hz, 1H), 7.24 (d, J=2.5 Hz, 1H), 6.65 (d, J=2.0 Hz, 1H), 5.33 (s, 2H), 4.95-4.93 (m, 1H), 4.39 (s, 2H), 3.52 (s, 3H), 1.38 (s, 9H).
WORKUP
后处理
- customThe mixture was evaporated in vacuo
- customthe residue was purified by reverse-phase prep-HPLC