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Methanol → Methyl 3-bromo-5-nitrobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3-Bromo-5-nitrobenzoic acid | HCID 239336 | — |
| 生成物 | Methyl 3-bromo-5-nitrobenzoate | HCID 239341 | 94% |
反応手順
To a solution of 3-bromo-5-nitro-benzoic acid (D5) (22.3 g, 90.6 mmol, 1 equiv) in MeOH (300 ml) at 0° C. was added SOCl2 (7.9 ml, 108 mmol, 1.2 equiv) dropwise. The resulting solution was stirred at reflux for 4 hours then cooled to room temperature and concentrated in vacuo. The residue was diluted with AcOEt, washed twice with 2N aqueous NaOH solution and once with brine, dried over MgSO4 and concentrated in vacuo to give 3-bromo-5-nitro-benzoic acid methyl ester (D11) (22.1 g, 94%) as a pale brown solid. RT=3.18 min
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07253198B2 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-af069a73802042128b68719f111f09ae |
| 出典メモ | uspto-grants-2007_08 |