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2-(3-Amino-2-nitro-phenylsulfanyl)-ethanol → 2-(2,3-Diamino-phenylsulfanyl)-ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(3-Amino-2-nitro-phenylsulfanyl)-ethanol | HCID 21877331 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2,3-Diamino-phenylsulfanyl)-ethanol | HCID 19044017 | 87% |
反応手順
2-(3-Amino-2-nitro-phenylsulfanyl)-ethanol (1.02 g, 4.8 mmol) was reduced by hydrogenation using 45 psi of H2 with 10% Pd—C (180 mg) in EtOAc (25 mL) for 6 h. After filtering through Celite, solvent was removed in vacuo. Purification by silica gel chromatography (EtOAc) gave 762 mg (87%) of 2-(2,3-diamino-phenylsulfanyl)-ethanol as a faintly yellow solid. 1H NMR (300 MHz, CDCl3) δ 6.98 (dd, 1H, J=7.5, 1.5 Hz), 6.60-6.72 (m, 2H), 3.65 (t, 2H, J=5.7 Hz), 3.55 (br s, 5H), 2.91 (t, 2H, J=5.7 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06534524B1 |
| 出典データセット | uspto-grants-2003_03 |
| ORD ID | ord-94eff58e540944218540db5f40c171c7 |
| 出典メモ | uspto-grants-2003_03 |