HRID1351212

反应详情

EQUATION

反应方程式

HRID 1351212 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 (5-allyl-6,7-dimethoxy-quinazolin-4-yl)-(3-chloro-4-fluoro-phenyl)-amine (0.102 g, 0.27 mmol) (from Example 18, Step E, supra) in dichloromethane (20 mL) was added I2 (0.69 g, 2.7 mmol). The reaction mixture was stirred at room temperature for 2 hours. The mixture was diluted with chloroform (100 mL) and washed with a saturated aqueous Na2SO3 solution. The organic layer was separated, dried over Na2SO4, and concentrated to give the desired 4-(3-chloro-4-fluoro-phenyl)-5-iodomethyl-7,8-dimethoxy-5,6-dihydro-4H-1,3,4-triaza-phenalene as a yellow foam. (Yield 0.134 g, 99%).

WORKUP

后处理

  1. washwashed with a saturated aqueous Na2SO3 solution
  2. customThe organic layer was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated