HRID722127

反应详情

EQUATION

反应方程式

HRID 722127 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe mixture was filtered
  2. filtrationAfter filtration