HRID921622

反应详情

EQUATION

反应方程式

HRID 921622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(I10A): A solution of 7-bromo-2,4-dichloroimidazo[2,1-f][1,2,4]triazine (Intermediate I9F)(10 g, 37.3 mmol) in anhydrous THF (300 ml) was treated with N-(4-methoxybenzyl)ethanamine (8.01 ml, 46.7 mmol), resulting in the immediate precipitation of a solid. The reaction was stirred for 1 hour; the mixture was concentrated in vacuo. To the residue was added EtOAc (100 ml) and the mixture stirred 10 min. The salts were filtered off and the filtrate was washed with 0.5M citric acid, sat. NaHCO3, water and brine. The solution was dried over Na2SO4 and solvents removed to afford 7-bromo-2-chloro-N-ethyl-N-(4-methoxybenzyl)imidazo[2,1-f][1,2,4]triazin-4-amine (15.8 g).

WORKUP

后处理

  1. customresulting in the immediate precipitation of a solid
  2. concentrationthe mixture was concentrated in vacuo
  3. additionTo the residue was added EtOAc (100 ml)
  4. stirringthe mixture stirred 10 min
  5. filtrationThe salts were filtered off
  6. washthe filtrate was washed with 0.5M citric acid, sat. NaHCO3, water and brine
  7. dry with materialThe solution was dried over Na2SO4 and solvents
  8. customremoved