反应详情

1.72 Grams of 3-hydroxy-4-cyano-5-methylthioisothiazole was dissolved in 20 ml of DMF, 0.7 g of potassium carbonate was added thereto, and then 1.3 g of propargyl bromide was added with stirring. After stirring at 50° C. for 1 hour, the reaction solution was ice-cooled, 3.0 g of iodine and 3.2 g of potassium iodide were added thereto, and then 6.6 g of a 10% KOH was gradually added dropwise with stirring. After addition, the reaction solution was stirred at room temperature for 1 hour. Water was added to the reaction solution to precipitate crystals, which were then collected by filtration and washed with water to obtain crude crystals. Recrystallization of the crude crystals from ether gave 2.5 g of crystals having a melting point of 145° to 146° C. (yield, 75%).

1. stirringAfter stirring at 50° C. for 1 hour
2. temperaturecooled
3. stirringwith stirring
4. additionAfter addition
5. stirringthe reaction solution was stirred at room temperature for 1 hour
6. customto precipitate crystals, which
7. filtrationwere then collected by filtration
8. washwashed with water
9. customto obtain crude crystals
10. customRecrystallization of the crude crystals from ether