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Methyl iodide → Tert-butyl 3-(3-chloro-2-fluorophenyl)-3-methoxypyrrolidin-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Tert-butyl 3-(3-chloro-2-fluorophenyl)-3-hydroxypyrrolidine-1-carboxylate | HCID 67404349 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl 3-(3-chloro-2-fluorophenyl)-3-methoxypyrrolidin-1-carboxylate | HCID 86658587 | 77% |
反応手順
Preparation according to Preparation 2. Tert-butyl-3-(3-chloro-2-fluorophenyl)-3-hydroxypyrrolidin-1-carboxylate (8.05 g, 25.5 mmol) in dry tetrahydrofuran (50 mL), sodium hydride (60% dispersion in mineral oil, 1.53 g, 38.2 mmol), iodomethane (3.17 mL, 51 mmol). Purification by flash column chromatography on silica gel (ethyl acetate/isooctane, 1:9 to 1:1) gave the title compound (6.45 g, 77%). MS m/z (rel. intensity, 70 eV) 256 (19), 228 (15), 199 (23), 187 (28), 57 (bp).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09035073B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-dd47010cb97049a185277f9977a539c0 |
| 出典メモ | uspto-grants-2015_05 |