참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Aminobenzonitrile | HCID 13396 | — |
| 반응물 | Heptafluorobutyryl Chloride | HCID 67810 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,2,3,3,4,4,4-heptafluoro-N-[4-(cyano)phenyl]butanamide | HCID 14253806 | 36.9% |
반응 단계
A mixture of 4-aminobenzonitrile (1.58 g), triethylamine (1.36 g), and dichloromethane (20 mL) was cooled in ice under a nitrogen atmosphere. To this mixture was added perfluorobutyryl chloride (3.11 g) in dichloromethane (10 mL) and the resulting mixture was allowed to warm to room temperature and was then stirred for three hours. The reaction mixture was diluted with HCl solution (1N, 50 mL) and the layers were partitioned in a separatory funnel. The organic phase was washed with a saturated brine solution, dried over MgSO4, filtered and concentrated with a rotary evaporator. The residue was dissolved in dichloromethane. Upon dilution with hexane the product precipitated to give 1.55 g of 2,2,3,3,4,4,4-heptafluoro-N-[4-(cyano)phenyl]butanamide, m.p. 116°-118° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04764623 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-fd7a1f957094494980469d14f25061e8 |
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| 출처 메모 | uspto-grants-1988_08 |
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