참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trifluoroacetonitrile | HCID 67710 | — |
| 반응물 | (2,4-Dichloro-5-(1-methylethoxy)phenyl)hydrazine | HCID 170281 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Pentane | HCID 8003 | — |
| 생성물 | HCID 178458719 | HCID 178458719 | 87.8% |
반응 단계
Under a dry nitrogen atmosphere a stirred solution of 2.4 g (0.01 mole) of 2,4-dichloro-5-(1-methylethoxy)phenylhydrazine in 140 mL of methanol was cooled to -60° C. in a dry ice-isopropanol bath. Trifluoroacetonitrile (23.2 g, 0.24 mole) was bubbled into the cold solution during a two minute period. After complete addition the cold solution was stirred for 30 minutes, then allowed to warm slowly to room temperature during the next three hours. A stream of nitrogen gas was bubbled into the room temperature solution to aid in the vaporization and removal of trifluoroacetonitrile, leaving a liquid residue. This residue was evaporated further under reduced pressure to leave a resinous material. This material was stirred in cold pentane to produce a solid. The pentane was decanted and the solid triturated in fresh cold pentane. The pentane was decanted and the solid dried under reduced pressure to yield 2.9 g of N-[2,4-dichloro-5-(1-methylethoxy)anilino]trifluoroacetamidine (mp 80.5°-81° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04919708 |
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| 출처 데이터셋 | uspto-grants-1990_04 |
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| ORD ID | ord-86946f2bc75e428e93b9c1b86fa90a84 |
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| 출처 메모 | uspto-grants-1990_04 |
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