反应 #2507855

反应方程式

2-(3,4-Dimethylphenyl)hydrazinium chloride

ethyl acetoacetate

sodium acetate

acetic acid

→

title compound

收率 71.0%

1-(3,4-dimethylphenyl)-3-methyl-1H-pyrazol-5-ol

收率 71.0%

溶剂

—

Petroleum ether

ethanol

反应条件

后处理

1. 1
   温度The resulting mixture was cooled
2. 2
   浓缩concentrated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane (10 L)
4. 4
   洗涤carefully washed with saturated sodium bicarbonate (3×3 L)
5. 5
   浓缩The organic layer was concentrated
6. 6
   其他to afford a solid
7. 7
   温度under reflux
8. 8
   温度the resulting mixture was cooled
9. 9
   过滤filtered

实验过程

2-(3,4-Dimethylphenyl)hydrazinium chloride (900 g, 5.21 mol), ethyl acetoacetate (678 g, 5.21 mol), sodium acetate (428 g, 5.21 mol) and glacial acetic acid (10 L) were stirred at 118° C. for about 24 hours. The resulting mixture was cooled and concentrated, and the residue was dissolved in dichloromethane (10 L) and carefully washed with saturated sodium bicarbonate (3×3 L). The organic layer was concentrated to afford a solid. The solid was dissolved in ethanol (450 mL) under reflux. Petroleum ether (7.2 L) was slowly added, and the resulting mixture was cooled and filtered to afford the title compound (748 g, 71%). PXRD analysis provided the diffractogram as shown in FIG. 31.

来源