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1-(3-Chloro-4-nitro-phenyl)-4-ethyl-piperazine → 2-Chloro-4-(4-ethyl-piperazin-1-yl)-phenylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-Chloro-4-nitro-phenyl)-4-ethyl-piperazine | HCID 69161998 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Chloro-4-(4-ethyl-piperazin-1-yl)-phenylamine | HCID 69253358 | — |
反応手順
A suspension of 1-(3-chloro-4-nitro-phenyl)-4-ethyl-piperazine (1 g, 3.7 mmol) and Raney Nickel (0.1 g) in MeOH (20 mL) is stirred for 8 h at RT, under a hydrogen atmosphere. The reaction mixture is filtered through a pad of celite and concentrated. The residue is purified by silica gel column chromatography (DCM/MeOH+1% NH3aq, 95:5) to afford the title compound as an off-white solid: ESI-MS: 240.1/242.1 [MH]+; tR=0.90 min (system 1), TLC: Rf=0.46 (DCM/MeOH+1% NH3aq, 95:5).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08293746B2 |
| 出典データセット | uspto-grants-2012_10 |
| ORD ID | ord-1b393b30d0a344b1a7e05774db7decb3 |
| 出典メモ | uspto-grants-2012_10 |