関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 2,4,6-Tribromophenoxyacetone | HCID 3303004 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Methyl-2-(2,4,6-tribromo-phenoxy)-ethylamine | HCID 45283177 | 32% |
反応手順
To a solution of 1 g 1-(2,4,6-tribromo-phenoxy)-propan-2-one (2.6 mmol) in 20 ml methanol is added 2.9 g ammonium acetate (39 mmol). The mixture is cooled to 0° C. and 0.81 g sodiumcyanoborohydride (13 mmol) is added. The reaction mixture is stirred overnight at ambient temperature. The completion of the reaction is confirmed by TLC. The reaction mixture is concentrated and the remaining residue is dissolved with 1.5 N HCl and washed with diethylether. The aqueous layer is neutralised and extracted with ethylacetate. The ethylacetate layer is dried over anhydrous sodium sulphate and the solvent removed. 0.32 g 1-methyl-2-(2,4,6-tribromo-phenoxy)-ethylamine (32%) is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08324263B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-a0968f2ae70d429b94778511187801b7 |
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| 出典メモ | uspto-grants-2012_12 |
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