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Hydrochloric Acid → 2-Chloro-5-nitrophenyl 3-chloro-2-thienyl ketone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Chlorothiophene | HCID 87017 | — |
| 反応物 | Benzoyl chloride, 2-chloro-5-nitro- | HCID 117637 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-5-nitrophenyl 3-chloro-2-thienyl ketone | HCID 20634258 | 44% |
反応手順
To a mixture of aluminum chloride (1.33 g, 0.0102 mol) and methylene chloride is added 3-chlorothiophene (1.21 g, 0.0102 mol) dropwise. The resultant mixture is stirred 30 minutes and treated with a solution of 2-chloro-5-nitrobenzoyl chloride (2.20 g, 0.0100 mol) in methylene chloride. The resultant mixture is stirred overnight at room temperature, poured into ice, acidified with concentrated hydrochloric acid and extracted twice with methylene chloride. The combined organic layers are washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to a brown oil. Trituration with ether affords the title compound as a brown solid (1.33 g, 44.0%, mp 114-116° C.) which is identified by NMR spectral analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706663B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-b88bd5e8fc374d8eaafcec445099e04a |
| 出典メモ | uspto-grants-2004_03 |