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Nitrofen → 4-(2,4-Dichlorophenoxy)benzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrofen | HCID 15787 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(2,4-Dichlorophenoxy)benzenamine | HCID 26940 | — |
反応手順
The nitro intermediate (10 mmol) obtained above was dissolved in MeOH (20 mL), and treated with SnCl2.2H2O (50 mmol), according to General Procedure I. The reaction mixture was heated under reflux until completion, as indicated by TLC or HPLC. The solvent was removed in vacuuo and the residue was treated with 4.0 N aqueous NaOH to pH ˜8. The residue was extracted with EtOAc (2×50 mL), washed with 1.0 N aqueous NaOH (50 mL), brine (50 mL) and dried over sodium sulfate. The solvent was removed in vacuuo to afford the desired 4-(2,4-dichloro-phenoxy)aniline, which was used directly for further transformation without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07714013B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-1c20915ecc344134be57b543f85d7785 |
| 出典メモ | uspto-grants-2010_05 |