関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Hydrazinopyridine | HCID 10909519 | — |
| 反応物 | Methyl 3-(3-chlorobenzoyl)-4-oxopentanoate | HCID 44247886 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Methyl 2-[5-(3-chlorophenyl)-3-methyl-1-(pyridin-3-yl)pyrazol-4-yl]acetate | HCID 24853498 | — |
反応手順
0.577 g (4.233 mmol) of 3-hydrazinopyridine in 5.00 ml of ethanol was added to 0.650 g (2.419 mmol) of methyl 3-(3-chlorobenzoyl)-4-oxopentanoate, and the mixture was stirred in a closed vessel in a microwave oven at 130° C. for 1.5 h. The solvent was removed under reduced pressure, and the residue was taken up in dichloromethane and washed twice with in each case 25 ml of water. The combined organic phases were dried over sodium sulfate, and the solvent was removed under reduced pressure. Chromatography of the residue gave 0.364 g (42% of theory) of a light-yellow oil. 1H-NMR (CDCl3): see Table 2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08252723B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-76739736b14c447e83fa235c27e92d13 |
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| 出典メモ | uspto-grants-2012_08 |
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