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4,5-Dichloro-2-nitrobenzaldehyde → 2-Amino-4,5-dichlorobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4,5-Dichloro-2-nitrobenzaldehyde | HCID 2749246 | — |
| 触媒 | Ferrous sulfate heptahydrate | HCID 62662 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-4,5-dichlorobenzaldehyde | HCID 818013 | 86.8% |
反応手順
3,4-Dichloro-6-nitrobenzaldehyde (4.40 g, 20 mmol) was dissolved in 50% aqueous ethanol (200 ml) at 50°-60° C. and the solution was added to a solution of iron(II) sulfate heptahydrate (27.8 g, 100 mmol) in water (200 ml) at 90° C. Concentrated (25%) aqueous ammonia (50 ml) was added in several portions with intensive stirring while the temperature was kept close to the boiling point. The mixture was refluxed for 5-10 min. and cooled. The precipitate was filtered off and washed with ethanol. The filtrate was concentrated in vacuo until most of the ethanol was removed. The resulting precipitate was collected, washed with water and dried in vacuo at 40°-50° C. to give 3.3 g of 3,4-dichloro-6-aminobenzaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05710139 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-2e39e3bdfd2e4393baa17f651f3c6417 |
| 出典メモ | uspto-grants-1998_01 |