関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 11-Bromoundecanoic acid | HCID 17812 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| 生成物 | N-methyl-11-bromoundecanohydroxamic acid | HCID 15035264 | — |
反応手順
According to the procedure shown in Example 11, 2.65 g (10 mmol) of 11-bromoundecanoic acid (IV5) was treated with 1 ml of thionyl chloride and the resulting product was treated with 850 mg (10.2 mmol) of methylhydroxylamine hydrochloride and 1.5 g (10.9 mmol) of potassium carbonate to give N-methyl-11-bromoundecanohydroxamic acid (V6), which was recrystallized from a mixture of ether-n-hexane to give 2.46 g of the compound (V6) as colorless prismatic crystals in 83.6% yield. mp. 49° C. to 51° C. To a solution of 2.11 g (7.2 mmol) of the compound (V6) was allowed to react with 1.71 g (7.2 mmol) of 3,5-di-tert-butyl-4-hydroxythiophenol under the condition shown in Example 11. The prepared product was chromatographed and eluted with a mixture of ether-ethyl acetate (2:1) to give 3.12 g of the aimed compound (I13) as a pale yellow in 96.3% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05091569 |
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| 出典データセット | uspto-grants-1992_02 |
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| ORD ID | ord-f54623565cef4901a18367f82765a24a |
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| 出典メモ | uspto-grants-1992_02 |
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