HRID1796657

反应详情

EQUATION

反应方程式

HRID 1796657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. washwashed with water (2×20 ml)
  2. dry with materialdried with Na2SO4
  3. concentrationConcentrated in vacuo
  4. custompurified by prep