HRID908253
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
A methanesulofonic acid 1.5 mL solution of the product from Step B (910 mg, 1.87 mmol) was stirred at 95° C. in an oil bath for 25 min. The reaction mixture was cooled to room temperature, diluted with MeCN—H2O (2:3) mixture (3 mL). The resulting solution was purified by reverse phase HPLC (C-18 column) (eluent: gradient mixture of acetonitrile-water with 0.5% TFA) to give the title compound (414 mg). LC/MS: m/z 423(M+H). 1H-NMR (d6-DMSO, 500 MHz): δ 5.59 (s, 2H), 7.06 (d, 1H), 7.35-7.39 (m, 4H), 7.61-7.68 (m, 3H), 7.93 (d, 1H), 13.14 (s, 1H).
WORKUP
后处理
- customThe resulting solution was purified by reverse phase HPLC (C-18 column) (eluent: gradient mixture of acetonitrile-water with 0.5% TFA)