HRID722127
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 stirred solution of ethyl 6-amino-9-(3-chlorobenzyl)-9H-β-carboline-3-carboxylate (139 mg, 0.37 mmol) in methanol (15 mL) under a nitrogen atmosphere were added NaOH (2N, 0.7 mL) and H2NOH (15 mL, 50 wt. % solution in H2O, 0.23 mol). The suspension was stirred for 7 days at ambient temperature and then diluted with H2O (10 mL). The mixture was filtered, and the solid was boiled in methanol (20 mL). After filtration, the title compound (36 mg, 27%) was obtained. 1H NMR (400 MHz, DMSO-d6): δ 11.17 (1H, s), 8.90–8.95 (2H, m), 8.55 (1H, s), 6.96–7.51 (7H, m), 5.72 (2H, s), 5.03 (2H, br, s). HRMS (M+H)+ found: 367.0961. Calcd for C19H16ClN4O2: 367.0962.
WORKUP
后处理
- filtrationThe mixture was filtered
- filtrationAfter filtration