反应 #42778

反应方程式

hydrazine hydrate

2,4,6-trimethylbenzenesulfonic acid 3-(4-chlorophenyl)-8-formyl-2-isopropyl-4-oxo-4H-chromen-7-yl ester

magnesium sulphate

ammonium acetate

→

3-(4-Chlorophenyl)-2-isopropyl-7H-pyrano[2,3-e]indazol-4-one

溶剂

ethanol

反应条件

后处理

1. 1
   其他The tube is sealed
2. 2
   温度The mixture is cooled to room temperature
3. 3
   其他the volatiles are evaporated under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue is dissolved in dry pyridine (14 ml)
5. 5
   其他the solution is transferred to a 20 ml microwave tube
6. 6
   其他the tube is sealed
7. 7
   温度the mixture is heated at 190° C. for 100 min
8. 8
   温度The mixture is cooled
9. 9
   其他evaporated to dryness
10. 10
    其他The residue is purified by chromatography on silica gel

实验过程

To a suspension of 2,4,6-trimethylbenzenesulfonic acid 3-(4-chlorophenyl)-8-formyl-2-isopropyl-4-oxo-4H-chromen-7-yl ester (391 mg, 0.745 mmol), magnesium sulphate (450 mg, 3.72 mmol) and ammonium acetate (230 mg, 2.98 mmol) in ethanol (15 ml) in a 20 ml microwave tube is added hydrazine hydrate (0.93 ml, 2.98 mmol). The tube is sealed and heated at 145° C. for ca. 80 min. The mixture is cooled to room temperature, and the volatiles are evaporated under reduced pressure. The residue is dissolved in dry pyridine (14 ml), the solution is transferred to a 20 ml microwave tube, the tube is sealed, and the mixture is heated at 190° C. for 100 min. The mixture is cooled and evaporated to dryness. The residue is purified by chromatography on silica gel using cyclohexane/ethyl acetate (6:1) as eluant.

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