HRID2239851

反应详情

EQUATION

反应方程式

HRID 2239851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

In a 2 dram reaction vial was added 8-bromo-6-chloroimidazo[1,2-b]pyridazine hydrochloric acid salt (0.5 g, 1.9 mmol) from Example I(1), step 1b, 4-nitroaniline (0.27 g, 1.9 mmol), 1.0 M potassium tert-butoxide in THF (7.6 ml, 7.6 mmol) and DMF (1.4 ml). Under N2, the reaction was stirred for 16 hr at 50° C. and the concentrated in vacuo. The resulting material was taken up in ethyl acetate and washed with H2O (2×50 ml) and then brine (1×20 ml). the organic layers were combined and dried over Na2SO4 and filtered. Following solvent evaporation, 0.42 g of crude 6-chloro-N-(4-nitrophenyl)imidazo[1,2-b]pyridazin-8-amine was obtained.

WORKUP

后处理

  1. customIn a 2 dram reaction
  2. concentrationthe concentrated in vacuo
  3. washwashed with H2O (2×50 ml)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customFollowing solvent evaporation