HRID1351223
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-(4-chloro-phenyl)-5,6-dihydro-4H-1,3,4-triaza-phenalen-5-ol (140 mg, 0.39 mmol) (from Example 21, Step A, supra) and triethylamine (0.32 mL, 2.33 mmol) in dichloromethane (50 mL) at 0° C. was added methanesulfonyl chloride (0.12 mL, 1.55 mmol) (Aldrich). The reaction solution was the 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-(4-chloro-phenyl)-7,8-dimethoxy-4H-1,3,4-triaza-phenalene as a yellow solid. (Yield 47 mg, 55%).
WORKUP
后处理
- concentrationThe solution was then concentrated
- customthe residue was purified by chromatography