関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzothiazole | HCID 7222 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Chloropropan-1-amine hydrochloride | HCID 145855 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Aminopropylthio)-aniline | HCID 20288563 | — |
反応手順
270 parts of benzothiazole and 160 parts of sodium hydroxide are boiled under reflux for 3 hours in 400 parts of water. After cooling to 70° C., 250 parts of methanol are added, followed by the dropwise addition over a period of 2 hours at 70° C. of a solution of 260 parts of 2-chloropropylamine·HCl in 500 parts of water. After stirring for another 3 hours at 100° C., the mixture is cooled and a solution of 100 parts of sodium hydroxide in 200 parts of water is added to it. The organic phase is separated off, the aqueous phase is washed twice with 200 parts of toluene and the combined organic phases are concentrated by evaporation, leaving 346 parts of 2-(3-aminopropylthio)-aniline in the form of a yellowish liquid boiling at 130° C./0.04 mm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04254229 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-a8eb211dc1a9495db2f7b22432defe2f |
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| 出典メモ | uspto-grants-1981_03 |
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