HRID65581

反应详情

EQUATION

反应方程式

HRID 65581 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Into a 1000 ml autoclave, are added 1-(2-thienyl)-2-propanol p-toluenesulfonate (75 g) and ammonia (600 ml). The whole is heated to 80° C. during 15 hours. After cooling, the autoclave is opened and the ammonia is allowed to evaporate. After adding water (100 ml) and a 1N sodium hydroxide solution (175 ml), the resulting material is extracted with ether. The ether phase is separated and then mixed with 1N hydrochloric acid (75 ml). The aqueous phase is made alkaline and is then extracted with ether. The ether extract is washed with a 5% sodium bicarbonate solution, and then with a saturated sodium chloride solution, after which it is dried over sodium sulfate. After evaporation, the residue is distilled in vacuo, to give 19 g 2-amino-1-(2-thienyl)-propane (Yield: 53%) boiling at 84°-86° C. under 12 mm Hg.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customto evaporate
  3. additionAfter adding water (100 ml)
  4. extractiona 1N sodium hydroxide solution (175 ml), the resulting material is extracted with ether
  5. customThe ether phase is separated
  6. additionmixed with 1N hydrochloric acid (75 ml)
  7. extractionis then extracted with ether
  8. extractionThe ether extract
  9. washis washed with a 5% sodium bicarbonate solution
  10. dry with materialwith a saturated sodium chloride solution, after which it is dried over sodium sulfate
  11. customAfter evaporation
  12. distillationthe residue is distilled in vacuo