HRID656401

反应详情

EQUATION

反应方程式

HRID 656401 的结构方程式

PROCEDURE

实验过程

To (±)-5′-amino-3-methyl-spiro[imidazolidine-4,2′-indane]-2,5-dione (100 mg, 0.432 mmol, described in Intermediate 7) at 0° C. were added 70% HNO3 (1 mL) followed by conc. H2SO4 (1 mL). The resulting mixture was allowed to warm to ambient temperature and stirred for 18 h, then poured onto ice and the precipitate was removed by filtration. The aqueous filtrate was purified by HPLC using a reversed phase C18 column and eluting with a gradient of H2O:CH3CN:CF3CO2H—90:10:0.1 to 5:95:0.1. Lyophilization provided the title compound. MS: m/z=277 (M+1).

WORKUP

后处理

  1. additionpoured onto ice
  2. customthe precipitate was removed by filtration
  3. customThe aqueous filtrate was purified by HPLC
  4. washeluting with a gradient of H2O