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1,1'-Carbonyldiimidazole → 2-(4-(4,9-diethoxy-1-oxo-1H-benzo[f]isoindol-2(3H)-yl)phenyl)-N-((4-fluorophenyl)sulfonyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Fluorobenzenesulfonamide | HCID 120231 | — |
| 反応物 | [4-(4,9-diethoxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetic acid | HCID 9931112 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-(4,9-diethoxy-1-oxo-1H-benzo[f]isoindol-2(3H)-yl)phenyl)-N-((4-fluorophenyl)sulfonyl)acetamide | HCID 9894082 | 35.3% |
反応手順
To a solution of carbonyldiimidazole (13.2 mg, 0.081 mmol) and [4-(4,9-diethoxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetic acid (30 mg, 0.074 mmol) in dichloromethane (2 ml) was added 4-fluorobenzenesulphonamide (14.3 mg, 0.081 mmol) and N,N-diisopropylethylamine (10.5 mg, 0.81 mmol). The mixture was stirred at ambient temperature under an atmosphere of nitrogen overnight. The reaction mixture was diluted with dichloromethane (3 ml) and then washed with 2N hydrochloric acid (5 ml). The organic phase was dried (MgSO4) and then concentrated in vacuo to give a brown gum. The residue was purified using mass directed autopurification to give the title compound as a white solid (14.7 mg, 35.3%). MH+563.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07173047B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-74fcd33b573a41169ca8bf9fead8c9a7 |
| 出典メモ | uspto-grants-2007_02 |