HRID1940594
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 7-amino-5-nitro-2,3-dihydrobenzofuran (D4) (2 g) in ethanol (60 ml) was treated with 2-dimethylaminoethyl chloride hydrochloride (3.36 g) and excess sodium carbonate (6 g), and heated at reflux for 4 days under argon. The solvent was evaporated under reduced pressure, and the residue partitioned between water and chloroform. The organic phase was dried (Na2SO4) and evaporated under reduced pressure to leave an oil which was chromatographed on silica, eluting with methanol and chloroform to give the title compound as a viscous red oil (416 mg, 15%)
WORKUP
后处理
- temperatureheated
- temperatureat reflux for 4 days under argon
- customThe solvent was evaporated under reduced pressure
- customthe residue partitioned between water and chloroform
- dry with materialThe organic phase was dried (Na2SO4)
- customevaporated under reduced pressure
- customto leave an oil which
- customwas chromatographed on silica
- washeluting with methanol and chloroform