関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide | HCID 20320282 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide | HCID 21444211 | — |
反応手順
To a stirred suspension of 876.0 g. (3.0 moles) of N,N,N,-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide in 2.75 liters of absolute methanol at room temperature is added a freshly prepared solution of sodium hydroxide (120.0 g., 3.0 moles) in 1.0 liter of absolute methanol over a period of 1.0 hour. The reaction mixture is evaporated under reduced pressure and the solid residue is shaken with 750 ml. of acetonitrile. The insoluble sodium bromide is removed by filtration and the filtrate is evaporated. The solid residue is dried in vacuo to give a quantitative yield of white, crystalline hygroscopic product which may be used without further purification or can be recrystallized from isopropanol-ether. NMR (D2O) δ: 2.28 (3H, S, --NHCH3); 3.11 (9H, S, --+N(CH3)3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04098726 |
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| 出典データセット | uspto-grants-1978_07 |
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| ORD ID | ord-b6dcb70210ef499da27dbd61b23b6722 |
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| 出典メモ | uspto-grants-1978_07 |
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