Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Amino-4,6-dimethoxypyrimidine | HCID 118946 | — |
| Reactant | Sodium Cyanate | HCID 517096 | — |
| Reactant | 1-methyl-4-ethoxycarbonylpyrazole-5-sulfonylchloride | HCID 10977963 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Pyrazosulfuron-ethyl | HCID 91750 | 98% |
Reaction Steps
7.27 g of anhydrous sodium cyanate, 15.78 g of 2-amino-4,6-dimethoxypyrimidine, 8.04 g of pyridine and 40 g of dry acetonitrile were mixed together and the mixture was warmed to 45° C. under nitrogen atmosphere. To this mixture was added 28.46 g of 1-methyl-4-ethoxycarbonylpyrazole-5-sulfonylchloride over 2 hours and the reaction mixture was stirred for further 2 hours while maintaining the temperature of 45° C. After the completion of the reaction was identified by liquid chromatography, the reaction product was extracted with 200 g of dichloromethane and 40 g of 5% aqueous sulfuric acid solution. The extracted organic layer was dried over anhydrous magnesium sulfate and then filtered. The organic solvent was removed from the product to obtain 41.30 g (Yield 98%) of the title compound as a solid state.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05480993 |
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| Source dataset | uspto-grants-1996_01 |
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| ORD ID | ord-b46e1e80933241f0a5c255e73e389dc5 |
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| Source note | uspto-grants-1996_01 |
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