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1,2-Dichloroethane → Formate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Chloro-p-anisic acid | HCID 169982 | — |
| 反応物 | HCID 44819544 | HCID 44819544 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Formate | HCID 283 | 423.1% |
| 生成物 | HCID 25054307 | HCID 25054307 | — |
反応手順
A reaction vial was charged with 3-chloro-4-methoxybenzoic acid (40 mg, 0.21 mmol), 3-aminomethyl-N-(4-dimethylaminomethyl-phenyl)-benzamide (40 mg, 0.14 mmol), EDC (40 mg, 0.25 mmol) and HOBt (40 mg, 0.29 mmol). DMF (2 mL) was added followed by Hunig's base (0.11 mL, 0.57 mmol). The mixture was stirred at room temperature for 16 h. The product was purified by preparative HPLC using an acetonitrile/water/formic acid gradient providing the title compound as a formate salt (20 mg, 31% yield); MS, electrospray, 452 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093266B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-332f0387552244a0a63ba1c192ea222c |
| 出典メモ | uspto-grants-2012_01 |