関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methylcyclohexane | HCID 7962 | — |
| 反応物 | Pentyl nitrite | HCID 10026 | — |
| 反応物 | 2',4'-Difluoropropiophenone | HCID 123586 | — |
| 生成物 | (2E)-1-(2,4-difluorophenyl)-2-hydroxyiminopropan-1-one | HCID 20609430 | 88.6% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06664422B1 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-cac912218ac44e9fa42236da914b3ae6 |
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| 出典メモ | uspto-grants-2003_12 |
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