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Sodium sulfate decahydrate → N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium sulfate decahydrate | HCID 62649 | — |
| 反応物 | N-(2,6-dichloro-4-cyanophenyl)acetamide | HCID 2735977 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide | HCID 58962993 | 30% |
反応手順
Step AT2. To a solution of 4-acetamido-3,5-dichloro-benzonitrile (114 mg, 0.5 mmol) in 5 mL of THF was added lithium aluminum hydride (120 mg, 3.2 mmol) in portion and the resulting mixture was stirred for 3 hours. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in portion and the mixture was stirred for 30 minutes. The solid was filtered off and the filtration was concentrated. Residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07612069B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-27e4930584df49deaf113f207d70c4b4 |
| 出典メモ | uspto-grants-2009_11 |