HRID408554
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
100 mg (1.026 mmol) cyclopentane-1,3-dione, 150 mg (1.026 mmol) 1H-indazole-5-carbaldehyde and piperidine (0.1 ml) in ethanol (8 ml) were heated to reflux for 4 h. The mixture was then evaporated to dryness, the remaining solid was dissolved in acetic acid (8 ml), and 84 mg (1.026 mmol) 3-aminobut-2-enenitrile were added. The solution was heated to reflux for 2 h. After cooling, the mixture was evaporated to dryness again, and the remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient) to yield 40 mg (13% of th.) of the title compound.
WORKUP
后处理
- temperatureto reflux for 4 h
- customThe mixture was then evaporated to dryness
- dissolutionthe remaining solid was dissolved in acetic acid (8 ml)
- temperatureThe solution was heated
- temperatureto reflux for 2 h
- temperatureAfter cooling
- customthe mixture was evaporated to dryness again
- customthe remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient)