関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,3'-(1,1,3,3-Tetramethyldisiloxane-1,3-diyl)bispropylamine | HCID 17181 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 1,3-Bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride | HCID 86753608 | 90% |
反応手順
In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a condenser, and a dropping funnel was placed 24.9 g (0.1 mole) of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane having a gas chromatography purity of 98.4%. 31.3 g (0.3 mole) of concentrated hydrochloric acid was dropwise added to the flask, and the resulting mixture was stirred at room temperature for 30 minutes. 300 g of isopropanol was added to the solution. The resulting mixture was heated under reduced pressure, and isopropanol was distilled off while conducting azeotropic distillation, to obtain a concentrated and dried product. The concentrated and dried product thus obtained was recrystallized from isopropanol to obtain 28.9 g (yield: 90%) of 1,3-bis(3-amino-propyl)-1,1,3,3-tetramethyldisiloxane dihydrochloride which is an acid addition salt.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05861085 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-3ee4890127fa4b50a6a7a34191b47ece |
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| 出典メモ | uspto-grants-1999_01 |
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