反应详情

2-(3,4,5-trimethoxyphenyl)-4-methyl-5-acetylthiazole prepared in Example 1 (1.0 g corresponding to its 0.0033 mol) was dissolved in 30 ml of ethanol, and to the solution, 8.6 ml of an aqueous 2% solution of sodium hydroxide (0.0045 mol) and 0.4 g (0.0044 mol) of thiosemicarbazide were added, and the mixture was heated for 3 hours under a reflux condenser. After cooling the reaction mixture, it was introduced into 300 ml of iced water, and the precipitate which separated was collected by filtration. After washing the precipitate with water, it was recrystallized from ethanol to obtain the object consisting of yellow needle-like crystals amounting to 0.82 g at a yield of 65%, which decomposed at 209° to 212° C.

1. temperaturethe mixture was heated for 3 hours under a reflux condenser
2. temperatureAfter cooling the reaction mixture, it
3. customthe precipitate which separated
4. filtrationwas collected by filtration
5. washAfter washing the precipitate with water, it
6. customwas recrystallized from ethanol
7. customto obtain the object
8. customdecomposed at 209° to 212° C.