HRID908263
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
- 100 °C
PROCEDURE
实验过程
To the product obtained in example 22 (40 mg, 0.083 mmol) suspended in H2O (0.5 mL) was added conc. HCl (0.68 mL, 8.31 mmol). The mixture was placed in a microwave reactor and heated to 100° C. for 10 min. Resulting suspension was diluted with 3:1 MeCN:H2O (2 mL) along with DMSO (1 mL) and purified by reverse phase HPLC (C-18 column) to give the title compound (29 mg). LC/MS: m/z 468(M+H). 1H-NMR (600 MHz, d6-DMSO): δ 5.45 (s, 2H), 6.98 (d, 1H), 7.32 (t, 2H), 7.53 (d, 1H), 7.61 (d, 1H), 7.88 (d, 1H), 8.15 (s, 1H), 8.17 (d, 1H), 8.71 (d, 1H).
WORKUP
后处理
- customThe mixture was placed in a microwave reactor
- customResulting suspension
- customH2O (2 mL) along with DMSO (1 mL) and purified by reverse phase HPLC (C-18 column)