関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (2-Chloro-5-nitrophenyl)acetonitrile | HCID 53396322 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Potassium Carbonate | HCID 11430 | — |
| 生成物 | 2-(5-Amino-2-chlorophenyl)acetonitrile | HCID 53396333 | 91.2% |
反応手順
To a suspended solution of (2-Chloro-5-nitro-phenyl)-acetonitrile (4.0 g, 20.0 mmol) in EtOH (10 mL) is added a solution of Sn(II)Cl2 (15.36 g, 81.0 mmol) in concentrated HCl (14 mL) at 75° C. After the mixture is stirred for 30 minutes at 75° C., the mixture is diluted with EtOAc and neutralized with K2CO3 until a pH of 8 is achieved. The organic layer is washed with saturated K2CO3, brine and dried, filtered and concentrated to give crude product, which is purified by recrystallization with CH2Cl2/EtOAc/Hexane to give the title intermediate as a solid (3.04 g, 89.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449582B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-ae2d1c4a708a4d2f8e3b0c0fc887c5e7 |
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| 出典メモ | uspto-grants-2008_11 |
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