HRID1099262

反应详情

EQUATION

反应方程式

HRID 1099262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled (0° C.) solution of 1-(4-aminopyrrolo[2,1-f][1,2,4]triazin-7-yl)ethanone (262.0 mg, 1.49 mmol) in DMF (21 mL) was added 1,3-dibromo-5,5-dimethylhydantoin (212.6 mg, 0.74 mmol). The mixture was stirred for 80 min and then quenched by addition of saturated aqueous sodium sulphite (10 mL) and water (60 mL). The mixture was allowed to warm to rt and the precipitate was collected by filtration. The solid was air-dried to yield 360.0 mg (95%) of the title compound. 1H-NMR (DMSO-d6) δ 9.49 (bs, 1H), 8.49 (bs, 1H), 8.12 (s, 1H), 7.64 (s, 1H), 2.56 (s, 3H); MS [M+H]+=255.3; LCMS RT=1.96 min.

WORKUP

后处理

  1. customquenched by addition of saturated aqueous sodium sulphite (10 mL) and water (60 mL)
  2. filtrationthe precipitate was collected by filtration
  3. customThe solid was air-dried