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Acetic Anhydride → N-[2-(2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethyl]acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethanamine | HCID 68698969 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | N-[2-(2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethyl]acetamide | HCID 68700363 | 82% |
反応手順
2-(2-Methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethanamine (400 mg, 1.88 mmol) was dissolved in tetrahydrofuran (19 mL), triethylamine (287 μL, 2.06 mmol) and acetic anhydride (195 μL, 2.06 mmol) were added under ice-cooling, and the mixture was stirred for 15 min. The reaction solution was diluted with saturated aqueous sodium hydrogen carbonate solution, diluted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→10/90) to give the title compound (393 mg, yield 82%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08247429B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-805bbc0badea412ba49fc5ee5984fb2d |
| 出典メモ | uspto-grants-2012_08 |