関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bentonite | HCID 71586775 | — |
| 反応物 | HCID 178508056 | HCID 178508056 | — |
| 溶媒 | 2,5-Hexanedione | HCID 8035 | — |
| 溶媒 | Dichloromethane methanol | HCID 21226129 | — |
| 生成物 | HCID 178425431 | HCID 178425431 | — |
反応手順
A mixture of 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (100 mg) and Montmorillonite KSF clay (100 mg) in acetonylacetone (1 ml) was heated at 120° C. (50 W) for 15 minutes in a CEM discover microwave synthesiser. The reaction mixture was diluted with 5% methanol/dichloromethane, filtered and evaporated. The crude product was purified by flash column chromatography eluting with 1:2 ethyl acetate/hexane, and the product containing fractions were combined and evaporated to give 65 mg of the target molecule as a pale brown solid. (LC/MS: Rt 3.75 [M+H]+ 299).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07745638B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-aa3be304f8654d67b5c9d429009d1f72 |
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| 出典メモ | uspto-grants-2010_06 |
|---|