HRID4362

反应详情

EQUATION

反应方程式

HRID 4362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of N-amino-4-phenyl-1,2,3,6-tetrahydropyridine hydrochloride (1.05 g) in a mixture of dioxane (10 ml) and water (5 ml) was added 1N sodium hydroxide solution (5 ml) under ice-bath cooling, and then a solution of 4-fluorophenyl isothiocyanate (1.15 g) in dioxane (5 ml) was added thereto. The mixture was stirred for 5 hours under ice-bath cooling. The reaction mixture was evaporated in vacuo and the residue was extracted several times with ethyl acetate. The combined extract was washed with water, dried over magnesium sulfate and evaporated in vacuo to give a crude product, which was recrystallized from ethyl acetate to give N-[[(4-fluorophenyl)thiocarbamoyl]amino]-4-phenyl-1,2,3,6-tetrahydropyridine (1.05 g).

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. customThe reaction mixture was evaporated in vacuo
  4. extractionthe residue was extracted several times with ethyl acetate
  5. extractionThe combined extract
  6. washwas washed with water
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo
  9. customto give a crude product, which
  10. customwas recrystallized from ethyl acetate