関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | [2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazine | HCID 688223 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N'-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide | HCID 22015908 | 91% |
反応手順
A solution of chloroacetyl chloride (2.3 ml, 1.08 equivalents) in anhydrous dichloromethane (30 ml) was added during 30 minutes to a stirred solution of 2,6-dichloro-4-trifluoromethylphenylhydrazine (6.1 g, 24.89 mmol) in anhydrous dichloromethane (60 ml) maintaining between 5 and 12° C. under an argon atmosphere. The mixture was then stirred for 5-12 hours at 20° C. A solution of sodium hydroxide (11.2 ml of 10%) and dichloromethane were added and the organic phase washed (water), dried (magnesium sulfate) and evaporated to give the title compound (7.25 g) as a white solid, NMR 4.05 (s, 2H), 6.77 (s, 1H), 7.47 (s, 2H), 8.6 (s, 1H). The yield was 91%.
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-dfa9e18eb14e412c912226bdf971231a |
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| 出典メモ | uspto-grants-2006_08 |
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