関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pentaerythritol | HCID 8285 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 3-Mercaptobutyric acid | HCID 9964084 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Pentaerythritol tris(3-mercaptobutyrate) | HCID 54578067 | 47% |
反応手順
A 200 ml three-necked flask was charged with 15.0 g (110.2 mmol) of pentaerythritol (manufactured by TOKYO CHEMICAL INDUSTRY CO., LTD.), 26.5 g (220.3 mmol) of 3-mercaptobutanoic acid (manufactured by YODO KAGAKU CO., LTD.), 1.8 g (9.3 mmol) of p-toluenesulfonic acid monohydrate (manufactured by JUNSEI CHEMICAL CO., LTD.) and 35 g of toluene (manufactured by JUNSEI CHEMICAL CO., LTD.). A Dean-Stark apparatus and a condenser tube were attached. The materials were heated in an oil bath at 130° C. with stirring. After 4 hours after the reaction was initiated, 13.3 g (110.1 mmol) of 3-mercaptobutanoic acid was added. Further, 0.85 g (4.5 mmol) of p-toluenesulfonic acid monohydrate was added after 6 hours from the initiation of the reaction. The reaction was carried out for another 4 hours. The reaction liquid was allowed to cool, was neutralized with 200 ml of a saturated aqueous sodium hydrogen carbonate solution, and was washed twice with 200 ml of pure water. The reaction liquid was then dehydrated and dried over anhydrous magnesium sulfate (manufactured by JUNSEI CHEMICAL CO., LTD.) and was distilled to remove the toluene, thereby giving a mixture containing the target compound. PE3MB obtained was a colorless transparent liquid and weighed 22.5 g, providing 47% yield. The composition formula of PE3MB was C17H30O7S3 and the molecular weight was 442.61.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08053167B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-7bb5aba4008d4c34823c0305217766b5 |
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| 出典メモ | uspto-grants-2011_11 |
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