HRID1619366
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
A solution of methyl 2-amino-4-bromobenzoate (1.0 g, 4.34 mmol, 1 eq) and 4,5-dichloro-1,2,3-dithiazolium chloride (2.0 g, 9.6 mmol, 2.2 eq) in DCM (20 mL) was stirred at rt under N2 for 5 days. The reaction mixture was quenched with water and filtered. The filtrate was extracted with ethyl acetate (3×100 mL). The combined organic layers were dried over Na2SO4. After filtration and concentration, the residue was purified by silica gel chromatography to give the desired product. MS (ESI): 365, 367 (MH+).
WORKUP
后处理
- customThe reaction mixture was quenched with water
- filtrationfiltered
- extractionThe filtrate was extracted with ethyl acetate (3×100 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationAfter filtration and concentration
- customthe residue was purified by silica gel chromatography