関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclopropyl methyl ketone | HCID 13004 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Methyl 2-(methylthio)-4-(trifluoromethyl)benzoate | HCID 10944828 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Cyclopropyl-3-(2-methylthio-4-trifluoromethylphenyl)-1,3-propanedione | HCID 11120178 | 92.9% |
反応手順
Sodium methoxide (3.51 g. 0.065M) was added to a mixture of methyl 2-methylthio-4-trifluoromethylbenzoate (12.5 g 0.050M) and cyclopropyl methyl ketone (7 ml, 0.070M) in toluene. The mixture was heated at 55-57° C. for 1 hour. Methanol was distilled under reduced pressure. After cooling to 20° C. the mixture was acidified and the organic phase washed (sodium bicarbonate solution and with water) and evaporated to give 1-cyclopropyl-3-(2-methylthio-4-trifluoromethylphenyl)propane-1,3-dione as yellow crystals (14.03 g), m.p. 64° C. A yield of 92.9% was obtained. The purity of the product was 95%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06486356B2 |
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| 出典データセット | uspto-grants-2002_11 |
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| ORD ID | ord-6a83322701324a0384b901be95b17a33 |
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| 出典メモ | uspto-grants-2002_11 |
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