関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-Chlorobenzoylacetonitrile | HCID 2734201 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178507276 | HCID 178507276 | 88.4% |
反応手順
To a solution of 3-(chlorophenyl)-3-oxo-propionitrile (4.0 g, 22.2 mmol) in absolute ethanol (21 mL) was added hydrazine hydrate (6.5 mL, 134 mmol). The reaction mixture was stirred at 80° C. for 15 hours, then it was concentrated in vacuo and purified on silica gel with 0-10% MeOH in CH2Cl2 as eluent to give 3.8 g (87% yield) of 5-amino-3-(2-chlorophenyl)pyrazole as a yellow solid. 1H NMR (d6-DMSO) δ: 11.7 (broad s, 1H), 7.66 (d, 1H), 7.48 (d, 1H), 7.35 (t, 1H), 7.30 (t, 1H), 5.83 (s, 1H), 4.84 (broad s, 2H); HPLC/MS m/z: 194.1 [MH]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07473783B2 |
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| 出典データセット | uspto-grants-2009_01 |
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| ORD ID | ord-4a18ad9ee1e041b895ca8bc2150a214b |
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| 出典メモ | uspto-grants-2009_01 |
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