참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3-(Dimethylamino)prop-2-enenitrile | HCID 97497 | — |
| 반응물 | (4-Nitrophenyl)hydrazine | HCID 3310889 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1-Propanol | HCID 1031 | — |
| 생성물 | 16459-44-2 | HCID 12678771 | — |
반응 단계
7.65 g (50 mmol) of 4-nitrophenylhydrazine was suspended in 70 mL of water and 10 mL of n-propanol and the suspension was heated to about 50° C. At this temperature, 5 g (50 mmol) of concentrated hydrochloric acid and 4.81 g (50 mmol) of 3-dimethylaminoacrylonitrile were then added. After an additional 15 minutes, 3.8 mL (50 mmol) of a 25% ammonia solution was added dropwise within 15 minutes. The reaction mixture was then allowed to agitate at about 50° C. until the 3-dimethylaminoacrylonitrile had completely reacted (about 1 hour) after which the resulting dark-brown suspension was cooled in an ice bath. The precipitate was filtered off, washed 3 times with small portions of cold water and then dried. Yield of crude product: 9.4 g (46 mmol. 92% of the theoretical).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07195649B2 |
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| 출처 데이터셋 | uspto-grants-2007_03 |
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| ORD ID | ord-6bac166120524a40b37f69db9f43e5ef |
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| 출처 메모 | uspto-grants-2007_03 |
|---|