関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Dichlorobenzaldehyde | HCID 6737 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzaldehyde, 2,6-dichloro-, oxime | HCID 91328 | 99.6% |
反応手順
Sodium hydroxide 3N (3.14 L, 9.43 mol) is added dropwise to a stirred suspension of hydroxylamine hydrochloride (675.55 g, 9.43 mol) in 0.5 L of water at 0° C. To this mixture is added dropwise a suspension of 2,6-dichlorobenzaldehyde (1500 g, 8.57 mol) in 7.5 L of ethanol and the reaction is heated at 90° C. overnight. The mixture is cooled to room temperature and then, concentrated to dryness. The solid is triturated in a mixture of H2O/EtOH, 10:1 (4.4 L), filtered and dried under high vacuum at 45° C. overnight. 1621.78 g of title compound (99% yield) is obtained as a white solid. MS (m/e): 190 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08153624B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-c3f0e80f6181496680572301a72f489f |
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| 出典メモ | uspto-grants-2012_04 |
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