硫酸二甲酯-13C2,D6 → 3,4,5-tribroMo-1-Methyl-1H-pyrazole
反应方程式
[Br:1][C:2]1[C:6]([Br:7])=[C:5]([Br:8])[NH:4][N:3]=1.[OH-].[Na+].S(OC)(O[CH3:15])(=O)=O>>[Br:1][C:2]1[C:6]([Br:7])=[C:5]([Br:8])[N:4]([CH3:15])[N:3]=1参与物
4
实验过程
To 3,4,5-tribromopyrazole (4.5 g, 0.15 mole) in 3N aqueous sodium hydroxide (6 g, 0.15 mole) is added at room temperature with stirring dimethyl sulfate (19 g, 0.15 mole). After 10 minutes a solid separates out. An additional gram of dimethyl sulfate is added and the mixture is stirred for 3 days, filtered and the precipitate water washed and air dried to yield 33 g (73%), mp 85° C. to 86° C. Crystallization from cyclohexane yields desired solid product whose melting point ranges from about 90° C. to 91° C.
后处理
- filtrationfiltered
- washthe precipitate water washed
- customair dried
- customto yield 33 g (73%), mp 85° C. to 86° C
- customCrystallization from cyclohexane
- customyields desired solid product whose
- customranges from about 90° C. to 91° C.
来源与证据
- ORD记录
- ord-21bde602aead465ab7761bc39910ca12
- 来源数据集
- uspto-grants-1977_10
- 专利号
- US04053610
反应笔记
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