반응 #93306

반응 방정식

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

N-methylthiourea

triethylamine

→

4-(4-methoxyphenyl)-2-methylamino-5-(3-pyridyl)-1,3-thiazole

수율 85.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred for three hours
2. 2
   온도at refluxing temperature
3. 3
   기타the solvent was evaporated off
4. 4
   workup.ADDITIONTo the residue was added a saturated aqueous solution of sodium hydrogen carbonate
5. 5
   추출The mixture was subjected to extraction with ethyl acetate
6. 6
   기타The extract was dried
7. 7
   기타the solvent was evaporated off
8. 8
   기타The residue was recrystallized from ethyl acetate isopropyl ether

실험 절차

In 18 ml of acetonitrile was dissolved 242 mg of N-methylthiourea. In the solution was suspended 1.0 g of 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide. To the suspension was added dropwise slowly 0.4 ml of triethylamine while stirring. The mixture was stirred for three hours at refluxing temperature, and the solvent was evaporated off. To the residue was added a saturated aqueous solution of sodium hydrogen carbonate. The mixture was subjected to extraction with ethyl acetate. The extract was dried, then the solvent was evaporated off. The residue was recrystallized from ethyl acetate isopropyl ether to yield 650 mg (85%) of 4-(4-methoxyphenyl)-2-methylamino-5-(3-pyridyl)-1,3-thiazole, m.p. 158°-159° C.

출처