反应详情

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.

1. stirringThe mixture was stirred for three hours
2. temperatureat refluxing temperature
3. customthe solvent was evaporated off
4. additionTo the residue was added a saturated aqueous solution of sodium hydrogen carbonate
5. extractionThe mixture was subjected to extraction with ethyl acetate
6. customThe extract was dried
7. customthe solvent was evaporated off
8. customThe residue was recrystallized from ethyl acetate isopropyl ether