HRID557303

反应详情

EQUATION

反应方程式

HRID 557303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,3-dinitro-4-tert-butylbenzene (10.0 g) in H2O (56 ml) was heated to reflux. A mixture of Na2S (21.42 g) and sulfur (2.85 g) in H2O (34 ml) was added over 1 h via an addition funnel. The reaction maintained at reflux for 1.5 h then cooled to RT and extracted with EtOAc. The organic extracts were combined and washed with H2O, brine, dried over MgSO4 and concentrated in vacuo to afford 4-tert-butyl-3-nitro-phenylamine which was used as is without further purification.

WORKUP

后处理

  1. temperaturewas heated to reflux
  2. additionwas added over 1 h via an addition funnel
  3. temperatureThe reaction maintained
  4. temperatureat reflux for 1.5 h
  5. extractionextracted with EtOAc
  6. washwashed with H2O, brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo