反应详情

A reaction mixture of 5.25 g. of 3-dimethylaminoacrylophenone [von H. Meerwein et al., Annalen der Chemie, Band 641, 1-39, (1961)] and 2.50 g. of 3-aminopyrazole in 25 ml. of glacial acetic acid is refluxed for 3.5 hours, cooled overnight and evaporated to a thick yellow oil. This oil is dissolved in methylene chloride, washed with a saturated aqueous solution of sodium bicarbonate, dried over sodium sulfate and then passed through a sintered glass funnel or a chromatographic column packed in vacuo with hydrous magnesium silicate. Additional methylene chloride is passed through the funnel (column). The effluent is refluxed on a steam bath. The gradual addition of hexane produces crystals. The crystallization from methylene chloride with hexane is repeated giving the desired product, m.p. 72°-73° C.

1. additionA reaction mixture of 5.25 g
2. temperaturecooled overnight
3. customevaporated to a thick yellow oil
4. dissolutionThis oil is dissolved in methylene chloride
5. washwashed with a saturated aqueous solution of sodium bicarbonate
6. dry with materialdried over sodium sulfate
7. custompassed through a sintered glass funnel
8. temperatureThe effluent is refluxed on a steam bath
9. additionThe gradual addition of hexane
10. customproduces crystals
11. customThe crystallization from methylene chloride with hexane