Реакция #413270

Уравнение реакции

toluene

β-(2-methyl-6-phenyl-imidazo[2,1-b]-1,3,4-thiadiazol-5-yl)-propenoic acid

thionyl chloride

2-ethylpiperidine

→

N-[β-(2-Methyl-6-phenyl-imidazo[2,1-b]-1,3,4-thiadiazol-5-yl)-propenoyl]-2-ethyl-piperidine

Условия реакции

Обработка

1. 1
   Другоеa clear solution resulting
2. 2
   ТемператураThe solution was then heated
3. 3
   Температураunder reflux for 2 hours
4. 4
   Температураunder reflux for one hour
5. 5
   ФильтрацияThe cooled mixture was filtered (the residue
6. 6
   Экстракцияwas extracted twice with 300 ml of water
7. 7
   СушкаThe toluene phase was dried over sodium sulphate
8. 8
   Фильтрацияfiltered
9. 9
   Концентрированиеthe filtrate was concentrated by distillation
10. 10
    ДругоеThe residue was recrystallised from 400 ml of ethyl acetate

Методика

143 g (0.5 mole) of β-(2-methyl-6-phenyl-imidazo[2,1-b]-1,3,4-thiadiazol-5-yl)-propenoic acid were suspended in 1.5 liters of absolute toluene at 60° to 70° C. 50 ml of thionyl chloride were added dropwise, a clear solution resulting. The solution was then heated under reflux for 2 hours and subsequently cooled to room temperature. 220 ml (1.5 moles) of 2-ethylpiperidine were next added dropwise and the mixture was boiled under reflux for one hour. The cooled mixture was filtered (the residue was discarded) and the filtrate was extracted twice with 300 ml of water. The toluene phase was dried over sodium sulphate and filtered and the filtrate was concentrated by distillation. The residue was recrystallised from 400 ml of ethyl acetate.

Источник