関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Perchloric Acid | HCID 24247 | — |
| 反応物 | Piperazine, hexahydrate | HCID 120181 | — |
| 反応物 | Potassium Perchlorate | HCID 516900 | — |
| 反応物 | Piperazine perchlorate | HCID 85529587 | — |
| 反応物 | p-Dihydroxy benzene disulfonic acid potassium salt | HCID 131710108 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Bis (piperazine) p-dihydroxy benzene disulfonate | HCID 21151652 | — |
反応手順
To an aqueous solution of perchloric acid, containing 200 g of said acid in 500 ml of water 40 % solution, the amount of aqueous solution of piperazine hexahydrate required for neutralization is added. The required amount of piperazine hexahydrate is 388.46 g (C4H10N2.6H2O) dissolved in 500 ml of water. Preferably the pH of the neutralizing solution is controlled to a pH close to 6. The piperazine perchlorate solution is mixed with the warm solution of p-dihydroxy benzene disulfonic acid potassium salt, and is stirred until a copious precipitate of potassium perchlorate is formed, which then increases when the solution is left to cool for several hours. After filtering off the potassium perchlorate, the solution of a piperazine p-dihydroxy benzene disulfonate is concentrated in a rotary evaporator, under vacuum, at 60°C, until crystals begin to form, and it is then left in a refrigerator. The product is filtered and recrystallized in water to give 388 g of bis (piperazine) p-dihydroxy benzene disulfonate, having a melting point of 270°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03947448 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-e3e431b72b86492a8ce5a0f0bb48441c |
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| 出典メモ | uspto-grants-1976_03 |
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