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Diisopropylethylamine → 4-[2-(3-Bromo-4-chloro-benzoylamino)-phenyl]-butyric acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methyl 4-(2-aminophenyl)butanoate | HCID 237256 | — |
| 反応物 | 3-Bromo-4-chlorobenzoyl chloride | HCID 20229730 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[2-(3-Bromo-4-chloro-benzoylamino)-phenyl]-butyric acid methyl ester | HCID 68602147 | 101.9% |
反応手順
To 3-bromo-4-chloro-benzoyl chloride (1.09 g, 4.3 mmol) in DCM (30 mL) cooled with an ice bath, was added 4-(2-amino-phenyl)-butyric acid methyl ester (0.85 g, 4.4 mmol), followed by addition of diisopropylethylamine (1 mL, 5.6 mmol) slowly. Upon the completion of the addition, ice bath was removed and the mixture was stirred at room temperature for 12 hrs. The mixture was further diluted with DCM, washed with saturated NaHCO3, 1N HCl, brine and dried over Na2SO4 and concentrated to yield 4-[2-(3-bromo-4-chloro-benzoylamino)-phenyl]-butyric acid methyl ester (1.8 g). MS [M+H]+: 411.7; tR=2.45 min. (method 1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09422310B2 |
| 出典データセット | uspto-grants-2016_08 |
| ORD ID | ord-68351de091e246ce87bde63f435e25f8 |
| 出典メモ | uspto-grants-2016_08 |