関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodoacetonitrile | HCID 69356 | — |
| 反応物 | 5-Chloro-2-isopropyl-4-methoxy-phenol | HCID 59598668 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (5-Chloro-2-isopropyl-4-methoxy-phenoxy)-acetonitrile | HCID 59598662 | 97% |
反応手順
To a solution of 5-chloro-2-isopropyl-4-methoxy-phenol (10.36 g, 51.6 mmol) in 40 mL DMF was added K2CO3 (8.55 g, 62.0 mmol) and the mixture was heated to 65° C. After 15 minutes iodoacetonitrile (9.05 g, 54.2 mmol) was added and the mixture was heated to 80° C. for 1 hour. The mixture was cooled, poured into an ice/H2O mixture and extracted with 1:1 toluene/hexane. The combined organics were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by passing through a short plug of silica to afford (5-chloro-2-isopropyl-4-methoxy-phenoxy)-acetonitrile (11.97 g, 97%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524725B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-8b70b4f1efbc458fbfbd3492f9d230dc |
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| 出典メモ | uspto-grants-2013_09 |
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