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Hydrochloric Acid → 2-Amino-4-cyano-3-hydroxynitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrazinium, 1,1,1-trimethyl-, iodide (1:1) | HCID 18683 | — |
| 反応物 | 2-Hydroxy-4-nitrobenzonitrile | HCID 286148 | — |
| 反応物 | CID 131725183 | HCID 131725183 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-Amino-4-cyano-3-hydroxynitrobenzene | HCID 21875462 | — |
反応手順
Compound 477A (0.438 g, 2.67 mmol) was dissolved in 25 mL of DMSO and trimethylhydrazinium iodide (0.534 g, 2.67 mmol) was added. Sodium pentoxide (0.880 g, 8.01 mmol) was added under N2 to give a deep red solution and stirring was continued overnight at rt. The reaction mixture was poured into 50 mL of 10% HCl and extracted with EtOAc (2×25 mL). The combined organic layers were washed with water (25 mL), brine (25 mL), dried over sodium sulfate and concentrated in vacuo to give compound 477B as an oily red solid which was used directly in the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06953679B2 |
| 出典データセット | uspto-grants-2005_10 |
| ORD ID | ord-95cdb00792634fedb43a506ae15bc5e7 |
| 出典メモ | uspto-grants-2005_10 |