HRID2306579
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3,6-Dichloro-4-cyclobutylpyridazine (10 g, 0.049 mol) and hydrazine hydrate (14 ml, 0.30 mol) were heated at reflux in dioxan (125 ml) for 24 hours. Upon cooling the desired isomer crystallized from the reaction and was collected by filtration (4.8 g, 49%). 1H NMR (250 MHz, d6-DMSO) δ 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
- temperatureUpon cooling the desired isomer
- customcrystallized from the reaction
- filtrationwas collected by filtration (4.8 g, 49%)