Dimethyl Sulfate → 3,4,5-Tribromo-1-methyl-1H-pyrazole
Reaktionsgleichung
[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]=1Komponenten
4
Versuchsvorschrift
To 3,4,5-tribromopyrazole (4.5 g, 0.15 mole) at 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 (0.0079 mole) 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° to 86° C. Crystallization from cyclohexane gives desired solid product whose melting point ranges from 90° to 91° C.
Aufarbeitung
- filtrationfiltered
- washthe precipitate water washed
- customair dried
- customto yield 33 g (73%), mp 85° to 86° C
- customCrystallization from cyclohexane
- customgives desired solid product whose
- customranges from 90° to 91° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-b7ec2cc4e17c4489ba15992fb5f1843b
- Quelldatensatz
- uspto-grants-1977_08
- Patentnummer
- US04044013
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