Реакция #1674589

Уравнение реакции

1,2-bis(4-methoxyphenyl)-2-chloroethanone

N-diaminomethylenethiourea

water

→

4,5-bis(4methoxyphenyl)-2-guanidinothiazole

Выход 53.3%

Растворители

ethanol

Условия реакции

Обработка

1. 1
   Температураwas refluxed for 12 hours
2. 2
   Экстракцияextracted with ethyl acetate
3. 3
   ПромывкаThe separated organic layer was washed with water and brine
4. 4
   Сушкаdried over magnesium sulfate
5. 5
   Другоеevaporated in vacuo
6. 6
   ДругоеThe residue was chromatographed n alumina
7. 7
   Промывкаeluting with a mixture of chloroform and methanol
8. 8
   Концентрированиеconcentrated in vacuo
9. 9
   ПромывкаThe residue was washed with isopropy ether

Методика

A mixture of 1,2-bis(4-methoxyphenyl)-2-chloroethanone (1.00 g) and N-diaminomethylenethiourea (0.65 g) in ethanol (20 ml) was refluxed for 12 hours. After allowing to cool to ambient temperature, then the reaction mixture was poured into water and extracted with ethyl acetate. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed n alumina, eluting with a mixture of chloroform and methanol. The desired fractions were combined and concentrated in vacuo. The residue was washed with isopropy ether to give 4,5-bis(4methoxyphenyl)-2-guanidinothiazole (0.65 g).

Источник