関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 2,2,3,3,4,4,4-heptafluoro-N-[4-(2-cyanoethyl)phenyl]butanamide | HCID 21297708 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178522035 | HCID 178522035 | 43.3% |
反応手順
A mixture of 2,2,3,3,4,4,4-heptafluoro-N-[4-(2-cyanoethyl)phenyl]butanamide (3.9 g), sodium azide (3.7 g), ammonium chloride (3 g) and dimethylformamide (60 mL) was stirred under a nitrogen atmosphere and heated in a 130° C. oil bath for 48 hours. Water (300 mL) was added to the hot mixture to dissolve all suspended salts and the solution was allowed to cool to room temperature. More water was added and the precipitate was collected by filtration. The tan solid was dried at 65° C. in vacuo overnight and recrystallized from a hexane/tetrahydrofuran mixture to give 1.9 g (43% yield) of the title compound as a tan solid, m.p. 161°-162° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04764623 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-9153dc27639e4a4bb14481582c20460a |
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| 出典メモ | uspto-grants-1988_08 |
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