HRID1796657
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 3-cyano-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazine-6-carbonyl chloride (Example 412B) (181 mg, 0.45 mmol) in CH2Cl2 (3 ml) was added Et3N (160 μl, 1.13 mmol) followed by O,N-dimethylhydroxyamine hydrochloride (44 mg, 0.45 mmol) in one portion. The mixture was stirred overnight, diluted with CHCl3 (20 ml), washed with water (2×20 ml), dried with Na2SO4. Concentrated in vacuo and purified by prep. TLC to give the title compound (138 mg, 72%) (50% EtOAc—hexanes). It has a retention time of 6.45 min (standard LCl method, 8 min run). LCMS Found: (M+H)+=428.1
WORKUP
后处理
- washwashed with water (2×20 ml)
- dry with materialdried with Na2SO4
- concentrationConcentrated in vacuo
- custompurified by prep