関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Benzonitrile | HCID 7505 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178418369 | HCID 178418369 | 90.1% |
反応手順
Zinc chloride (3.3 g, 24.3 mmol, 0.5 eq) was added to 15 mL of N,N-dimethylformamide in small portions while maintaining the temperature below 60° C. The suspension of zinc chloride was cooled to room temperature and treated with 5.0 g of benzonitrile (48.5 mmol, 1.0 eq) followed by 3.2 g of sodium azide (48.5 mmol, 1.0 eq). The heterogeneous mixture was heated at 115° C. with agitation for 18 hours. The mixture was cooled to room temperature, water (30 mL) was added and the mixture acidified by the addition of 5.1 mL of concentrated hydrochloric acid. The mixture was cooled to 0° C. and aged for one hour, then filtered and the filter cake washed with 15 mL of cold 0.1N HCl then dried at 60° C. under vacuum to afford 6.38 g (43.7 mmol, 90%) of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05726319 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-683f6b06ba0444c18452d135760784ee |
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| 出典メモ | uspto-grants-1998_03 |
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