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Methylhydrazine → 3-Bromo-n-[4-chloro-2-(n-methylhydrazinocarbonyl)-6-methylphenyl]-1-(3-chloro-2-pyridinyl)-1h-pyrazole-5-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylhydrazine | HCID 6061 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 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 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-n-[4-chloro-2-(n-methylhydrazinocarbonyl)-6-methylphenyl]-1-(3-chloro-2-pyridinyl)-1h-pyrazole-5-carboxamide | HCID 66854276 | — |
反応手順
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:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07867949B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-b489a85920f742cb902c1886561fd5d7 |
| 出典メモ | uspto-grants-2011_01 |