関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1-ethyl-5-(4-hydroxybutyl)-1H-pyrazole-3-carboxamide | HCID 66958760 | — |
| 生成物 | 5-(4-chlorobutyl)-1-ethyl-1H-pyrazole-3-carbonitrile | HCID 66958967 | — |
反応手順
A modification of the method described in Part E of Examples 1-4 was used to treat 1-ethyl-5-(4-hydroxybutyl)-1H-pyrazole-3-carboxamide (18.2 g, 86.1 mmol) with phosphorous oxychloride (60 mL). The reaction was heated for three hours before cooling to 0° C. and pouring into ice water. The mixture was adjusted to pH 12 with the addition of 2 N aqueous sodium carbonate and extracted with chloroform. The combined extracts were passed through a layer of silica gel (eluting first with chloroform and then with 1:1 hexane/ethyl acetate to provide 10.8 g of 5-(4-chlorobutyl)-1-ethyl-1H-pyrazole-3-carbonitrile as a dark oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07544697B2 |
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| 出典データセット | uspto-grants-2009_06 |
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| ORD ID | ord-4c347ddfbb054590b7905470dd8abe46 |
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| 出典メモ | uspto-grants-2009_06 |
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