HRID1270597
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 5-(2,6-dichloro-4-nitro-phenoxy)-2-methoxy-(cyclopropyl-methane-sulfonyl)-benzene (160 mg, 0.37 mmol) in CH2Cl2 (3 mL) was added boron tribromide (1M in CH2Cl2, 0.74 mL, 0.74 mmol). The resulting mixture was stirred at room temperature for 2 h and water (15 mL) was added. After stirring at room temperature for 1 h, the solution was extracted with EtOAc (3×20 mL). The combined organic extracts were dried and concentrated. The residue was purified by preparative TLC (100% CH2Cl2) to afford the title compound of Step D (76 mg). MS (APCI−) Calc.: 417.0, Found: 416.2 (M−1).
WORKUP
后处理
- stirringAfter stirring at room temperature for 1 h
- extractionthe solution was extracted with EtOAc (3×20 mL)
- customThe combined organic extracts were dried
- concentrationconcentrated
- customThe residue was purified by preparative TLC (100% CH2Cl2)