関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Octabenzone | HCID 15797 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-(2-Hydroxy-3-diethylaminomethyl-5-tert-octylphenyl)-2H-benzotriazole | HCID 15219414 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2(Benzotriazol2yl)4tert-octyl-6-(2hydroxy-3-benzoyl-6-n-octyloxybenzyl)phenol | HCID 19917267 | 62% |
反応手順
Methanol (50 ml) is placed into a 300 ml three-necked flask equipped with a stirrer, thermometer, condenser, Dean-Stark trap and nitrogen inlet. Sodium (0.3 g, 0.013 mol) is added to the methanol and the mixture stirred at room temperature till all the sodium is dissolved. Then, 2-(2-hydroxy-3-diethylaminomethyl-5-tert-octylphenyl)-2H-benzotriazole (10.2 g, 0.025 mol), 2-hydroxy-4-n-octyloxybenzophenone (8.2 g, 0.025 mol) and another 50 ml of methanol are added to the sodium methoxide solution. The reactants are heated at reflux till half the methanol is collected in the Dean-Stark trap. o-Xylene (50 ml) is added and the temperature is raised to the reflux temperature of o-xylene (143°-145° C.) and heating is continued for 24 hours. The mixture is then cooled and acetic acid is added to neutralize the sodium methoxide catalyst. The o-xylene solvent is then removed by vacuum distillation. The crude product obtained is recrystallized from heptane to afford the title compound in a yield of 10 g (62 % yield) as a white crystalline solid melting at 96°-100° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05439955 |
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| 出典データセット | uspto-grants-1995_08 |
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| ORD ID | ord-c7c2b6cc19c040ddbb04ca435116aa01 |
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| 出典メモ | uspto-grants-1995_08 |
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