HRID380322

反应详情

EQUATION

反应方程式

HRID 380322 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,6-Dichloro-4-cyclobutylpyridazine (22.5 g, 0.11 mol) and hydrazine hydrate (34 ml, 0.66 mol) were heated at reflux in dioxane (280 ml) for 24 hours. Upon cooling the desired isomer crystallized from the reaction and was collected by filtration (13.3 g, 64%). 1H NMR (250 MHz , d6-DMSO) 1.68-1.86 (1H, m), 2.00-2.11 (3H, m), 2.29-2.38 (2H, m), 3.52-3.61 (1H, m), 4.35 (2H, br), 6.99 (1H, s), 8.06 (1H, br); MS (ES+) m/e 198 [MH]+, 200 [MH]+.

WORKUP

后处理

  1. temperatureUpon cooling the desired isomer
  2. customcrystallized from the reaction
  3. filtrationwas collected by filtration (13.3 g, 64%)