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
To a solution of 2-(4-(trifluoromethyl)benzyl-8-chloro-7-(4-chlorophenyl)-2H-[1,2,4]triazolo[4,3-b]pyridazin-3-one (16.5 mg, 0.376 mmol) prepared as described in Example 359, in 0.3 mL of DMF at RT, potassium carbonate (19.4 mg, 0.14 mmol) was added followed by phenol (13.2 mg, 0.14 mmol). The mixture was stirred for 4 h. After this time, the reaction mixture was diluted with 5 mL of 1N aqueous sodium hydroxide. The precipitate was collected by filtration and washed with 1N aqueous NaOH, and water. The solid was dried to the title compound, 2-(4-(trifluoromethyl)benzyl-7-(4-chlorophenyl)-8-phenoxy-2H-[1,2,4]triazolo[4,3-b]pyridazin-3-one (15.8 mg) as light yellow solid. HPLC RT: 4.02 min; MS, M+H=497; 1H NMR (CDCl3): δ 8.21 (s, 1H), 7.52-6.97 (m, 13H), 5.12 (s, 2H).
WORKUP
后处理
- filtrationThe precipitate was collected by filtration
- washwashed with 1N aqueous NaOH, and water
- dry with materialThe solid was dried to the title compound