関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isooctan-1-ol | HCID 15450 | — |
| 反応物 | Dibutyltin oxide | HCID 61221 | — |
| 反応物 | 2-(3'-tert-Butyl-2'-hydroxy-5'-(2-methoxycarbonylethyl)phenyl)benzotriazole | HCID 93481 | — |
| 生成物 | Octyl 3-(3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyphenyl)propanoate | HCID 9868461 | — |
反応手順
Methyl 3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate (353 g, 1 mol), isooctanol (260 g, 2 mol, from Exxon) and dibutyltin oxide (0.5 g, 0.002 mol) are charged to a reaction flask and heated to 175° C. While heating to 175° C., a 300 mm Hg vacuum is applied. After holding at 175° C. for 30 minutes, the excess isooctanol is distilled by slowly reducing the pressure to <5 mm Hg. The desired product is cooled and discharged. The title compound is obtained in a yield of 451 g (100%) as a light yellow oil whose structure is verified by 1Hnmr and mass spectroscopy. The non-distilled product is analyzed by ICP (Inductively Coupled Plasma) for tin and is found to contain 170 ppm of tin.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06740132B2 |
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| 出典データセット | uspto-grants-2004_05 |
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| ORD ID | ord-5a243d321e1a4a03b6a0ee57399bedda |
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| 出典メモ | uspto-grants-2004_05 |
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