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Dimethylformamide → Methyl 3-carbamoyl-5-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1,3-Benzenedicarboxylic acid, 5-nitro-, 1-methyl ester | HCID 74776 | — |
| 生成物 | Methyl 3-carbamoyl-5-nitrobenzoate | HCID 3741295 | 85% |
反応手順
A mixture of 3-methoxycarbonyl-5-nitrobenzoic acid (44 mmol), SOCl2 (40 mL) and DMF (1 mL) was heated to reflux for 2 hours. Then the excessive SOCl2 was removed under reduced pressure. The residue was dissolved in DCM (80 mL), and added with NH3.H2O (15 mL) dropwise after cooling by ice-water. After addition, it was continued to stir 5 min. The resulting mixture was filtrated to give methyl-3-carbamoyl-5-nitrobenzoate in 85% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07868001B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-4ff90498172a4076bdb23340aa885828 |
| 出典メモ | uspto-grants-2011_01 |