関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Thiosulfate ion | HCID 1084 | — |
| 反応物 | Sodium Thiosulfate Pentahydrate | HCID 61475 | — |
| 反応物 | Cyclohexane, 1,4-bis(chloromethyl)- | HCID 69992 | — |
| 反応物 | N-(1,1-Dimethylethyl)benzenemethanamine | HCID 76908 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | hexamethylene bis(thiosulphate)N-tert-butyl-N-benzylammonium salt | HCID 131714228 | — |
反応手順
1,4-bis(chloromethyl)cyclohexane (0.165 mole), sodium thiosulphate pentahydrate (0.369 mole) sodium sulfite (6.1 g), methanol (150 ml) and water (150 ml) were charged into an autoclave and heated at 135° C. for 45 minutes. To the cooled reaction mixture, which was a solution of 1,4-dimethylcyclohexane-α,α-bis(thiosulphate)sodium salt, 400 ml of water was added. N-tert-butylbenzylamine (0.306 mole) in 150 ml methanol and 850 ml H2O was adjusted with concentrated HCl to pH4, and the resulting solution was added with stirring to the thiosulphate solution. The white precipitate was filtered, washed with water and dried. Yield: 92 g, (91%) of 1,4-dimethylcyclohexane-α,α-bis(thiosulphate)N-tert-butyl, N-benzylammonium salt.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04520154 |
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| 出典データセット | uspto-grants-1985_05 |
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| ORD ID | ord-32b8be04b6174a2580d656012a7d1254 |
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| 出典メモ | uspto-grants-1985_05 |
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