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Triethylamine → 3-Bromo-5-(4-chloro-butanoylamino)-benzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 反応物 | Methyl 3-amino-5-bromobenzoate | HCID 18763420 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Bromo-5-(4-chloro-butanoylamino)-benzoic acid methyl ester | HCID 69356939 | 79.2% |
反応手順
To a solution of 3-amino-5-bromo-benzoic acid methyl ester (D12) (460 mg, 2.0 mmol, 1 equiv) in CH2Cl2 (10 ml) at room temperature was added NEt3 (306 μl, 2.2 mmol, 1.1 equiv) then 4-chlorobutyrylchloride (247 μl, 2.2 mmol, 1.1 equiv). The resulting mixture was stirred at room temperature for 16 h and then diluted with AcOEt. The organic phase was washed with 2N aqueous HCl solution, dried over MgSO4 and concentrated in vacuo to give 3-bromo-5-(4-chloro-butanoylamino)-benzoic acid methyl ester (D13) (530 mg, 79%) as a pale yellow oil. RT=2.88 s
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-61589f157084404b848ad049e39ea209 |
| 出典メモ | uspto-grants-2007_08 |