HRID358952
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 2-nitro-N-tert-butylaniline (37 g) and triethylamine (35 ml) in tetrahydrofuran (400 ml) was added dropwise a solution of ethoxalyl chloride (25 ml) in tetrahydrofuran (50 ml). The mixture was then brought to reflux temperature for 8 h. The solvent was removed by evaporation, and the residue was partitioned between ether (300 ml) and water (500 ml). The organic phase was washed twice with water, dried over Na2SO4 and evaporated. This left the title compound as light yellow crystals, m.p. 73°-74° C.
WORKUP
后处理
- temperatureto reflux temperature for 8 h
- customThe solvent was removed by evaporation
- customthe residue was partitioned between ether (300 ml) and water (500 ml)
- washThe organic phase was washed twice with water
- dry with materialdried over Na2SO4
- customevaporated
- waitThis left the title compound as light yellow crystals, m.p. 73°-74° C.