HRID358952

反应详情

EQUATION

反应方程式

HRID 358952 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 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

  1. temperatureto reflux temperature for 8 h
  2. customThe solvent was removed by evaporation
  3. customthe residue was partitioned between ether (300 ml) and water (500 ml)
  4. washThe organic phase was washed twice with water
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. waitThis left the title compound as light yellow crystals, m.p. 73°-74° C.