참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Sodium Azide | HCID 33557 | — |
| 반응물 | 2,2,3,3,4,4,4-heptafluoro-N-[4-(2-cyanoethyl)phenyl]butanamide | HCID 21297708 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178522035 | HCID 178522035 | 43.3% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04764623 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-9153dc27639e4a4bb14481582c20460a |
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| 출처 메모 | uspto-grants-1988_08 |
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