HRID969693

反应详情

EQUATION

反应方程式

HRID 969693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4,4-dimethyl-7-{2-[(pyridazin-4-ylmethylene)-amino]-benzoylamino}-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (Example 121, Step B, 200 mg, 0.41 mmol) in EtOAC (1 mL). Concentrated HCl in EtOAc (2 mL) was added. The reaction was stirred for 5 h under N2 atmosphere at RT. The solid was filtered off and dissolved in water. The aqueous solution was basified to pH 11-14 using 5 N NaOH. The resulting precipitate was filtered, washed with water and dried under vacuum, to obtain the titled compound as a tan solid. MS (ES+): 388.0 (M+H)+. Calc'd for C23H25N5O: 387.21.

WORKUP

后处理

  1. filtrationThe solid was filtered off
  2. dissolutiondissolved in water
  3. filtrationThe resulting precipitate was filtered
  4. washwashed with water
  5. customdried under vacuum