関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 2,4-dichloro-N-(1-hydroxy-2-methylpropan-2-yl)-6-methoxybenzamide | HCID 12802882 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(2,4-Dichloro-6-methoxyphenyl)-4,4-dimethyl-2-oxazoline | HCID 12802883 | 70% |
反応手順
N-(2-Hydroxy-1,1-dimethylethyl)-2,4-dichloro-6-methoxybenzamide (5.5 g, 18.8 mmol) was treated dropwise with thionyl chloride (5.5 ml) and stirred magnetically at 20° C. for 30 min. Dry ether (100 ml) was added, the mixture was stirred for an additional one hour and the oxazoline hydrochloride precipitate was collected by filtration. The salt was neutralized with 20% sodium hydroxide to afford an alkaline mixture which was extracted with ether. The ethereal extract was dried (MgSO4) and concentrated to give an oil (3.6 g, 70%), which crystallized on standing, mp 47°-50° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04567289 |
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| 出典データセット | uspto-grants-1986_01 |
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| ORD ID | ord-a96dc604fb3f41d39140d97f7fc8443a |
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| 出典メモ | uspto-grants-1986_01 |
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