HRID712156
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 stirred solution of 1,2-dibromo-3,5-dinitrobenzene (723 g, 2.22 mol) in MeOH (7.5 L) at rt was added potassium thiocyanate (431 g, 4.44 mol) and the resulting reaction mixture stirred under a nitrogen atmosphere for 16 h. The reaction mixture was then filtered and washed with methanol. The filtrate was concentrated at 30-33° C. under reduced pressure. The residue thus obtained was purified over silica gel (2-6% EtOAc-hexane) to obtain the desired product (549 g, 81%).
WORKUP
后处理
- customthe resulting reaction mixture
- filtrationThe reaction mixture was then filtered
- washwashed with methanol
- concentrationThe filtrate was concentrated at 30-33° C. under reduced pressure
- customThe residue thus obtained
- customwas purified over silica gel (2-6% EtOAc-hexane)