関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide | HCID 22015908 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazonoyl chloride | HCID 86591113 | 90% |
反応手順
Phosphoryl chloride (500 microlitres, 1.7 equivalents) was added in one portion to a stirred solution of N′-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide (1.0 g, 3.11 mmol) in toluene (20 ml) and heated at 70° C. under an argon atmosphere for 20 hours. The cooled mixture was evaporated and the residue extracted with cyclohexane. The extracts were combined and evaporated to give the title compound (0.971 g) as an orange oil, NMR 4.4 (s, 2H), 7.55 (s, 2H), 7.7 (s, 1H). The yield was 90%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087786B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-9a91687510384f2a99c8906dc00af77d |
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| 出典メモ | uspto-grants-2006_08 |
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