関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 5-Chlorovaleronitrile | HCID 80474 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178478463 | HCID 178478463 | — |
反応手順
100mmol of 5-chlorovaleronitrile are placed under an inert atmosphere in 100 ml of anhydrous tetrahydrofuran on an ice bath. 445 mmol of sodium azide and then 100 mmol of aluminum chloride are then added in small fractions. The reaction mixture is heated to 80° C. and left under reflux, with stirring, for 16 hours. The complex formed is then hydrolyzed by addition, dropwise, of 150 cm3 of 5% hydrochloric acid. The resulting aqueous phase is extracted with ethyl acetate and after washing the organic phase with water, then with a saturated sodium chloride solution, drying and evaporation, the residue obtained is taken up in pentane. The expected product is then obtained after filtration of the precipitate formed.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05561113 |
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| 出典データセット | uspto-grants-1996_10 |
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| ORD ID | ord-7c5079c0fe654c1b83febdf8eee3497c |
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| 出典メモ | uspto-grants-1996_10 |
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