반응 #4457

반응 방정식

N-amino-1,2,3,6-tetrahydropyridine hydrochloride

triethylamine

3-fluorophenyl isocyanate

→

N-[[(3-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine

수율 60.8%

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타the reaction mixture was evaporated to dryness
3. 3
   추출The residue was extracted with ethyl acetate (100 ml)
4. 4
   세척The extract was washed with water
5. 5
   기타evaporated to dryness

실험 절차

To a solution of N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (1.012 g) in dry methylene chloride (40 ml) was added a solution of 3-fluorophenyl isocyanate (1.37 g) in dry methylene chloride under ice-bath cooling. After stirring for one hour, the reaction mixture was evaporated to dryness. The residue was extracted with ethyl acetate (100 ml). The extract was washed with water, evaporated to dryness and recystallized from ethyl acetate to give N-[[(3-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine (1.43 g). mp: 136.5°-138.5° C.

출처