HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylhydrazine → 3-Bromo-n-[4-chloro-2-(n-methylhydrazinocarbonyl)-6-methylphenyl]-1-(3-chloro-2-pyridinyl)-1h-pyrazole-5-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylhydrazine | HCID 6061 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | 2-(3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazol-5-yl)-6-chloro-8-methyl-4H-benzo[d][1,3]oxazin-4-one | HCID 10253307 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-Bromo-n-[4-chloro-2-(n-methylhydrazinocarbonyl)-6-methylphenyl]-1-(3-chloro-2-pyridinyl)-1h-pyrazole-5-carboxamide | HCID 66854276 | — |
Reaktionsschritte
A mixture of 1.0 g of 2-[3-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazol-5-yl]-6-chloro-8-methyl-4H-3,1-benzoxazine-4-one, 0.35 ml of methylhydrazine and 20 ml of tetrahydrofuran was stirred at room temperature for 24 hours. Water was poured into the reaction mixture and the mixture was extracted with ethyl acetate three times. The combined organic layer was washed with an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.85 g of 3-bromo-N-[4-chloro-2-(N-methylhydrazinocarbonyl)-6-methylphenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxamide of the formula:
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07968573B2 |
| Quelldatensatz | uspto-grants-2011_06 |
| ORD ID | ord-b473d85cd6204416b515b847c2818522 |
| Quellennotiz | uspto-grants-2011_06 |