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Sodium Hydroxide → 1-(2-Benzothiazolylthio)-3-methyl-piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Methylpiperidine | HCID 79081 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 反応物 | HCID 178418395 | HCID 178418395 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(2-Benzothiazolylthio)-3-methyl-piperidine | HCID 21325669 | 95.5% |
反応手順
In a 500 ml volume flask, there are charged 2-mercaptobenzothiazole (UV absorption spectrum: 329 mμ) (41.28 g), sodium hydroxide (10 g) and water (180 ml), and the resultant mixture is stirred to form a solution. After the addition of 3-methylpiperidine (27.2 g) to the resulting solution, a 15 % by volume aqueous solution of sodium hypochlorite (138.5 ml) is dropwise added thereto in 2 hours, during which the inner temperature is kept below 70° C. The reaction mixture is allowed to stand at the same temperature for 1 hour and then shaken with ethyl acetate (150 ml). The ethyl acetate extract is washed with water and distilled under reduced pressure to give 1-(2-benzothiazolylthio)-3-methyl-piperidine (62.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04147696 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-365611d060fb4b2cbbb7eaf6a8fdb453 |
| 出典メモ | uspto-grants-1979_04 |