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6-Dimethylaminohexan-1-ol → Ammonium Hydroxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-Dimethylaminohexan-1-ol | HCID 74623 | — |
| 反応物 | Dodecane, 1-isocyanato- | HCID 77873 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | Dodecylcarbamic acid 6-(dimethylamino)hexyl ester | HCID 14407596 | — |
反応手順
1.1 gm (5 meq) of dodecyl isocyanate and 726 mg (5 meq) of 6-(dimethylamino)hexanol are combined in 5 ml of tetrahydrofuran and reacted over weekend at room temperature. The insoluble crystals are filtered, washed with ethyl acetate and the filtrate and washings combined, evaporated under reduced pressure (<30° C.) and dried in vacuo. The product is purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4). Fractions 34-46 are combined, evaporated and dried in vacuo to yield 300 mg (Rf 0.9 S.G. CH2Cl2, CH3OH, NH4OH) of title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04824996 |
| 出典データセット | uspto-grants-1989_04 |
| ORD ID | ord-10fe8ebfd8054af49d4995ba11d7035c |
| 出典メモ | uspto-grants-1989_04 |