反应详情

A mixture of 6.0g of tetrahydro-3,5-bis-[(4-chlorophenyl)methylene]-4H-thiopyran-4-one, 1.3g of n-propyl hydrazine, and 100mg of hydroquinone in 100ml of dichloroethane is heated at reflux temperature for 2.5 hours and allowed to cool to room temperature. The reaction mixture is washed with dilute hydrochloric acid and water, and then dried over calcium chloride. After the solvent is removed in vacuo, the residue is chromatographed on a dry packed neutral alumina column (Activity I). The fractions eluted with 0-5% ethyl acetate/hexane are combined and crystallized from acetone/acetonitrile to give 2.8g of the title compound, melting point 118°-122°C.

1. temperatureis heated
2. temperatureat reflux temperature for 2.5 hours
3. washThe reaction mixture is washed with dilute hydrochloric acid and water
4. dry with materialdried over calcium chloride
5. customAfter the solvent is removed in vacuo
6. customthe residue is chromatographed on a dry
7. washThe fractions eluted with 0-5% ethyl acetate/hexane
8. customcrystallized from acetone/acetonitrile