関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium bismuthate | HCID 4063671 | — |
| 反応物 | Methyl 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoate | HCID 18415839 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 4-(4-oxo-1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoate | HCID 9796477 | — |
反応手順
A mixture of methyl 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoate (6.3 g, Example 7), sodium bismuthate (31 g), glacial acetic acid (180 ml) and water (60 ml) was boiled under reflux for about 3.5 hours. A further amount of sodium bismuthate (33 g) was added and the mixture boiled under reflux for about 24 hours, then cooled. The pH of the reaction mixture was adjusted to 8-9 by addition of saturated sodium bicarbonate solution. The reaction mixture was filtered through a celite pad and the residue solid washed with ethyl acetate. The organic layer was separated, dried, filtered and evaporated to give a brown solid. The solid was boiled up in methanol (50 ml), cooled and the solid was filtered off, then dried to give methyl 4-(4-oxo-1,4-dihydroindeno[1,2-c]pyrazol-3-yl)benzoate, m.p. dec. 235° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06462036B1 |
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| 出典データセット | uspto-grants-2002_10 |
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| ORD ID | ord-4806c8fb898c481f9a233418259f6b1c |
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| 出典メモ | uspto-grants-2002_10 |
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