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Ethanol → HCID 58120261、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Benzene, 2,4-dichloro-1-fluoro- | HCID 123112 | — |
| 反応物 | (S)-3-((R)-2-Ethoxy-1-hydroxyethyl)pyrrolidine-1-carboxylic Acid t-Butyl Ester | HCID 66858889 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 58120261 | HCID 58120261 | — |
反応手順
(S)-3-((R)-2-Ethoxy-1-hydroxyethyl)pyrrolidine-1-carboxylic acid t-butyl ester (25.0 mg, 96.4 μmol) was dissolved in DMF (200 μL). NaH (2776 μg, 115.7 mmol) was added and the mixture was stirred at room temperature for 15 minutes. 2,4-Dichloro-1-fluorobenzene (22.6 μL, 192.8 μmol) was added and the mixture was stirred at 70° C. for 3 hours. The mixture was concentrated then dissolved in 1.2M HCl in EtOH (1.0 mL, 1.2 mmol) and stirred overnight. The product was concentrated and purified by preparative HPLC (10-40%, 60 min, BDS) to yield the title compound as a mono-TFA salt oil (24.4 mg, 100% purity). MS m/z: [M+H]+ calcd for C14H19Cl2NO2, 304.08. found 304.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08853255B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-0526e86200c448ec9adbf4cdf6810bbb |
| 出典メモ | uspto-grants-2014_10 |