HRID876838

反应详情

EQUATION

反应方程式

HRID 876838 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the ice-cooled mixture of N2-((1H-pyrrolo[2,3-b]pyridin-3-yl)methyl)-6-bromopyrazine-2,3-diamine (48 mg, 0.15 mmol) in HOAc/H2O (1.5 mL/1.5 mL) was added NaNO2 (31 mg, 0.45 mmol) in water (0.2 mL). The reaction was stirred for 1.5 h in an ice bath, then aqueous H2SO4 (49%, 0.1 mL) was added. The resulting mixture was allowed to warm to room temperature and stir overnight, then was adjusted to pH>8 with 3 N aqueous NaOH solution, and extracted with EtOAc. The combined organics were dried over Na2SO4, filtered and concentrated to give the title compound (46 mg) MS (m/z): 332 (M+1)+.

WORKUP

后处理

  1. stirringstir overnight
  2. extractionextracted with EtOAc
  3. dry with materialThe combined organics were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated