関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 3-Bromobenzonitrile | HCID 23381 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-Bromobenzene-1-carboximidamide hydrochloride | HCID 12207718 | — |
反応手順
1.18 g (22 mmol, 2 equiv.) ammonium chloride are suspended in 40 ml of dry toluene under an argon atmosphere, and the mixture is cooled to 0° C. 11 ml (22 mmol, 2 equiv.) of a 2M solution of trimethylaluminium in hexane are added dropwise, and the reaction mixture is stirred at room temperature until no more evolution of gas is observed. After addition of 2.0 g (11 mmol, 1 equiv.) 3-bromobenzonitrile, the mixture is stirred at 80° C. bath temperature over night. It is then cooled down to 0° C. and 50 ml of methanol are added with subsequent stirring of 1 hour at room temperature. After filtration, the solid is washed with methanol for several times, the solution is evaporated to dryness in vacuo and the residue washed with methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07087605B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-adc6fca9416e4444a84e843c2bdf93a5 |
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| 出典メモ | uspto-grants-2006_08 |
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