참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 1-ethyl-5-(4-hydroxybutyl)-1H-pyrazole-3-carboxamide | HCID 66958760 | — |
| 생성물 | 5-(4-chlorobutyl)-1-ethyl-1H-pyrazole-3-carbonitrile | HCID 66958967 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09145410B2 |
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| 출처 데이터셋 | uspto-grants-2015_09 |
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| ORD ID | ord-38ddf0678ed44cc6927b9fd76d2788c9 |
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| 출처 메모 | uspto-grants-2015_09 |
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