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o-Chloranil → ethyl 4-cyano-1,3-dimethyl-1H-indazole-5-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | o-Chloranil | HCID 73252 | — |
| 反応物 | ethyl 4-cyano-6,7-dihydro-1,3-dimethyl-1H-indazole-5-carboxylate | HCID 22402928 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | ethyl 4-cyano-1,3-dimethyl-1H-indazole-5-carboxylate | HCID 22402968 | 47.3% |
反応手順
A mixture of ethyl 4-cyano-6,7-dihydro-1,3-dimethyl-1H-indazole-5-carboxylate (13.5 g, 55.0 mmol), o-chloranil (16.3 g, 66.0 mmol) and dry benzene is stirred for 1.5 hours at reflux temperature, cooled and filtered. The filtrate is concentrated in vacuo, filtered through two pads of neutral alumina and evaporated to dryness to afford a yellow solid. Recrystallization from ethyl acetate affords the title product (6.33 g, 47.2%), mp 170°-175.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05516751 |
| 出典データセット | uspto-grants-1996_05 |
| ORD ID | ord-7e6ef78a7e6149acbb5ce549f8594c87 |
| 出典メモ | uspto-grants-1996_05 |