HRID619897

反应详情

EQUATION

反应方程式

HRID 619897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-aminothiophenol (90%, 100 g, 0.72 mol) and sodium hydroxide (31.7 g, 0.792 mol) in 90% aqueous ethanol (500 ml) was added dropwise 2-bromopropane (89 g, 0.72 mol) at room temperature. When the addition was complete, the reaction mixture was refluxed for 3 hours, cooled to room temperature, and then concentrated in vacuo. The residue was diluted with water (300 ml) and extracted with ether (3×500 ml). The ether extracts were washed with water and brine, dried with MgSO4 and concentrated in vacuo to yield the crude product. Distillation through a Vigreaux column gave 2-(1-methylethylthio)benzenamine: bp 94° (2.2-2.4 mm).

WORKUP

后处理

  1. additionWhen the addition
  2. temperaturethe reaction mixture was refluxed for 3 hours
  3. concentrationconcentrated in vacuo
  4. additionThe residue was diluted with water (300 ml)
  5. extractionextracted with ether (3×500 ml)
  6. washThe ether extracts were washed with water and brine
  7. dry with materialdried with MgSO4
  8. concentrationconcentrated in vacuo
  9. customto yield the crude product
  10. distillationDistillation through a Vigreaux column