반응 #93307

반응 방정식

2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)-ethanone hydrobromide

thiourea

triethylamine

→

2-amino-4-(4-methoxyphenyl)-5-(3-pyridyl)-1,3-thiazol

수율 90.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred for 3 hours at a refluxing temperature, which
2. 2
   workup.WAITwas then left standing
3. 3
   온도for cooling
4. 4
   기타Precipitating crystals
5. 5
   여과were collected by filtration
6. 6
   세척The crystals were washed with an aqueous solution of saturated hydrogen carbonate, water, ethanol and ethylether in that order
7. 7
   기타by drying
8. 8
   기타The crystals were recrystallised from tetrahydrofuran

실험 절차

In 40 ml of acetonitrile was dissolved 516 mg of thiourea. In the solution was suspended 2.5 g of 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)-ethanone hydrobromide. To the suspension was added dropwise slowly 0.95 ml of triethylamine while stirring. The mixture was stirred for 3 hours at a refluxing temperature, which was then left standing for cooling. Precipitating crystals were collected by filtration. The crystals were washed with an aqueous solution of saturated hydrogen carbonate, water, ethanol and ethylether in that order, followed by drying. The crystals were recrystallised from tetrahydrofuran to yield 1.5 g (90%) of 2-amino-4-(4-methoxyphenyl)-5-(3-pyridyl)-1,3-thiazol, m.p. 265°-266° C.

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