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Hydrochloric Acid → 5-benzyloxy-N1-methylbenzene-1,2-diamine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 5-benzyloxy-N-methyl-2-nitroaniline | HCID 67954051 | — |
| 触媒 | HCID 178503042 | HCID 178503042 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-benzyloxy-N1-methylbenzene-1,2-diamine hydrochloride | HCID 67953976 | 91% |
反応手順
5% platinum carbon (2.15 g, water content: 53.1%) was added to a toluene (300 mL) suspension of 5-benzyloxy-N-methyl-2-nitroaniline (20 g, 77.4 mmol), and catalytic hydrogenation reaction was performed at 4 atm. The reaction solution was filtered to remove a catalyst. The catalyst was washed with 2-propanol (40 mL), and the washing liquid was added to the precedent filtrate. Under ice cooling, concentrated hydrochloric acid (6.6 mL, 77.4 mmol) was added to the mixture, and the mixture was stirred under the same temperature for 30 minutes. The resulting precipitated crystals were collected by filtration, then washed with 2-propanol (60 mL), and dried at 50° C., thereby obtaining 18.6 g of a light-pink, crystal target compound (yield: 91%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08796447B2 |
| 出典データセット | uspto-grants-2014_08 |
| ORD ID | ord-fdbf1d2967f846c0bd4e9de657feda77 |
| 出典メモ | uspto-grants-2014_08 |