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O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine → 2-Oxo-octahydrocyclopenta[b]pyrrol-4-yl benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine | HCID 11830845 | — |
| 反応物 | 6-Oxobicyclo[3.2.0]heptan-2-yl benzoate | HCID 59259575 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Oxo-octahydrocyclopenta[c]pyrrol-4-yl benzoate | HCID 59259560 | — |
| 生成物 | 2-Oxo-octahydrocyclopenta[b]pyrrol-4-yl benzoate | HCID 59259571 | 133.4% |
反応手順
To a stirred solution of compound 1H (500 mg, 2.2 mmol) in CH2Cl2 (5 mL) was added a solution of O-mesitylenesulfonylhydroxylamine (650 mg, 3 mmol) in CH2Cl2 (2 mL) at −10° C., and the stirring was continued for 20 min between −10 to 0° C. It was concentrated, added to a mixed solvent of benzene and methanol (30 mL, 3:1) followed by a slurry of basic alumina (25 g) in methanol (20 mL). The reaction mixture was stirred at RT overnight, and alumina solid was removed by filtration. Purification by silica gel chromatography (5% to 100% EtOAc in hexanes, then 5% methanol in EtOAc) provide mixtures of the title compounds 1I and 1J (total 360 mg) as a yellow oil. MS (ES) m/z 246 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07696241B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-ff4911748c5a40cb91eab397b5486820 |
| 出典メモ | uspto-grants-2010_04 |