HRID1351225
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 7,8-dimethoxy-4-(3-bromo-phenyl)-5,6-dihydro-4H-1,3,4-triaza-phenalen-5-ol (0.17 g, 0.42 mmol) (from Example 22, Step A, supra) and triethylamine (0.35 mL, 2.53 mmol) in dichloromethane (30 mL) at 0° C. was added methanesulfonyl chloride (0.13 mL, 1.68 mmol) (Aldrich). The reaction solution was stirred at room temperature for 2 hours. The solution was then concentrated, the residue was purified by chromatography using EtOAc/CH2Cl2/NEt3 (1:1:0.01) as eluent to give the desired 4-(3-bromo-phenyl)-7,8-dimethoxy-4H-1,3,4-triaza-phenalene as an off white solid. (Yield 81 mg, 50%).
WORKUP
后处理
- concentrationThe solution was then concentrated
- customthe residue was purified by chromatography