HRID712156

反应详情

EQUATION

反应方程式

HRID 712156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe resulting reaction mixture
  2. filtrationThe reaction mixture was then filtered
  3. washwashed with methanol
  4. concentrationThe filtrate was concentrated at 30-33° C. under reduced pressure
  5. customThe residue thus obtained
  6. customwas purified over silica gel (2-6% EtOAc-hexane)