反应方程式
[NH2:1][C:2]1[C:3](=[O:15])[N:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:5]([CH3:8])[C:6]=1[CH3:7].[C:16]1([NH2:23])[CH:21]=[CH:20][CH:19]=[C:18]([NH2:22])[CH:17]=1.N.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>O>[NH2:23][C:16]1/[C:21](=[N:1]/[C:2]2[C:3](=[O:15])[N:4]([C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:5]([CH3:8])[C:6]=2[CH3:7])/[CH:20]=[CH:19][C:18](=[NH:22])[CH:17]=1参与物
6
实验过程
20 mmol of 4-amino-1,5-dimethyl-2-phenyl-1,2-dihydro-3H-pyrazol-3-one and 20 mmol of meta-phenylene diamine was dissolved in 30 g of an ice/water mixture and the pH was adjusted to 10 using 20 ml of 20% aqueous ammonia. While stirring, a solution of 24 mmol of ammonium persulfate in 10 ml of water was added dropwise over 30 minutes. The mixture was stirred at 0° C. for 1 h 30 min and the solid formed was separated by filtration and washed with water and acetone and dried in a desiccator under vacuum for 12 hours, which resulted in 1.8 g of expected product, or a yield of 30%.
后处理
- stirringThe mixture was stirred at 0° C. for 1 h 30 min
- customthe solid formed
- customwas separated by filtration
- washwashed with water and acetone
- customdried in a desiccator under vacuum for 12 hours
来源与证据
- ORD记录
- ord-8179a22236034f70bf4460853eb432f8
- 来源数据集
- uspto-grants-2009_09
- 专利号
- US07582123B2
关联笔记
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