関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | N-[3-(3-piperidinomethylphenoxy)propyl]phthalimide | HCID 12898565 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(3-(Piperidin-1-ylmethyl)phenoxy)propan-1-amine | HCID 10220561 | 78% |
反応手順
To a solution of 16.3 g of the N-[3-[3-(piperidinomethyl)phenoxy]propyl]phthalimide in 150 ml of methanol was added 2.3 g of hydrazine monohydrate, and the mixture was heated at 70° C. for 4 hours. The mixture was cooled, then the solvent was distilled off, 30 ml of 6N hydrochloric acid was added to the residue, and the mixture was heated at 60° C. for 15 minutes. The resulting mixture was cooled, the insolubles were then filtered off, the solution was made alkaline with potassium hydroxide and subjected to extraction with a mixture of ethyl acetate and diethyl ether (1:1), and the organic layer was dried over magnesium sulfate and thereafter distilled to remove the solvent, giving 8.3 g of pale yellow oily 3-[3-(1-piperidinomethyl)phenoxy]propylamine (yield 78% ).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05401739 |
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| 出典データセット | uspto-grants-1995_03 |
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| ORD ID | ord-9a144552368646b29bf16aa0e1e8441b |
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| 出典メモ | uspto-grants-1995_03 |
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