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3-Acetylamino-6-bromo-2-nitro-benzoic acid → Methyl 3-acetylamino-6-bromo-2-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Acetylamino-6-bromo-2-nitro-benzoic acid | HCID 11403903 | — |
| 反応物 | trimethylsilyldiazomethane Et2O | HCID 23159941 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 3-acetylamino-6-bromo-2-nitrobenzoate | HCID 11151255 | 66.4% |
反応手順
To a mixed solution of 3-(acetylamino)-6-bromo-2-nitrobenzoic acid (2.00 g, 6.60 mmol) in methanol (20 mL) and tetrahydrofuran (5 mL) was added 2M trimethylsilyldiazomethane/diethyl ether solution (10.6 mL, 21.1 mmol) under ice-cooling, and the mixture was stirred at room temperature for 5 days. The reaction solution was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=25/75→60/40) to give the title compound (1.39 g, yield 66%).
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-ab75b8843663424d92e2efdb870c0921 |
| 出典メモ | uspto-grants-2012_08 |