反应详情

温度

50 °C

To a solution of 8.9 g of 1-chloro-3-(2-cyanoethylthio)propanone in 100 ml of acetone is added 6.3 g of amidinothiourea and the reaction mixture is stirred at 50° C. for 9 hours. Also, the reaction mixture is concentrated under reduced pressure, made basic with saturated sodium carbonate solution, and extracted with chloroformmethanol (10:1) solution (170 ml×2). The combined organic layer is dried over anhydrous magnesium sulfate, and is concentrated in vacuo to give a solid, which is crystallized from acetone-hexane to afford 10.2 g of the title compound, m.p.: 125°-128° C.

1. concentrationAlso, the reaction mixture is concentrated under reduced pressure
2. extractionextracted with chloroformmethanol (10:1) solution (170 ml×2)
3. dry with materialThe combined organic layer is dried over anhydrous magnesium sulfate
4. concentrationis concentrated in vacuo
5. customto give a solid, which
6. customis crystallized from acetone-hexane