反应详情

A stirred solution of tetrahydro-3,5-bis[(3,4,5-trimethoxyphenyl)methylene]-4H-pyran-4-one (3.0 g, 6.5 mmole) and 2-amino-2-thiazoline (0.8 g, 7.8 mmole) in 75 ml of CHCl3 is heated at reflux for 44 hours. After cooling, the solution is filtered to remove a small amount of insoluble material. The solvent is evaporated to give an oily residue which solidifies when treated with a small amount of EtOH. The yield is 2.2 g, m.p. 166°-168°. Crystallization from 10 ml of MeCN gives 1.5 g (42%) of light yellow solid, m.p. 153°-155°. The m.p. of a sample of this material does not change when recrystallized from MeCN.

1. temperatureat reflux for 44 hours
2. temperatureAfter cooling
3. filtrationthe solution is filtered
4. customto remove a small amount of insoluble material
5. customThe solvent is evaporated
6. customto give an oily residue which
7. customCrystallization from 10 ml of MeCN
8. customgives 1.5 g (42%) of light yellow solid, m.p. 153°-155°
9. customrecrystallized from MeCN