참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methylcyclohexane | HCID 7962 | — |
| 반응물 | Pentyl nitrite | HCID 10026 | — |
| 반응물 | 2',4'-Difluoropropiophenone | HCID 123586 | — |
| 생성물 | (2E)-1-(2,4-difluorophenyl)-2-hydroxyiminopropan-1-one | HCID 20609430 | 88.6% |
반응 단계
To a solution of 170 g (1.00 mol) of 2,4-difluoropropiophenone in 200 g methylcyclohexane 37 g (1.01 mol) of gaseous hydrochloric acid is dosed over 3 hours at 0° C. Thereafter 120 g (1.04 mol) of pentylnitrite are added over a period 3 to 4 hours to the reaction mixture at +10° C. to +15° C. Following the end of the addition the batch is stirred for an hour at +10° C. to +15° C. during which time a suspension is formed. The reaction mixture is then cooled to 0° C. and stirred for a further hour. The product is isolated by filtration and the filter cake is washed with 75 g of methylcyclohexane at 0° C.: 176 g of (E)-1-(2,4-difluoro-phenyl)-propane-1,2-dione-2-oxime (m.p. 99-101° C.) are obtained in 88.6% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06664422B1 |
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| 출처 데이터셋 | uspto-grants-2003_12 |
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| ORD ID | ord-cac912218ac44e9fa42236da914b3ae6 |
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| 출처 메모 | uspto-grants-2003_12 |
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