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Sodium hydride → tert-Butyl 3-(2-fluoroethoxy)-4,4-dimethoxypiperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Fluoroethyl p-Toluenesulfonate | HCID 256019 | — |
| 反応物 | Tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate | HCID 11425480 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | tert-Butyl 3-(2-fluoroethoxy)-4,4-dimethoxypiperidine-1-carboxylate | HCID 86648640 | 97.7% |
反応手順
The same operation as in Example (90a) was performed using tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate (6.2 g, 23.7 mmol), sodium hydride (55% content, 1.57 g, 36 mmol), 2-fluoroethyl p-toluenesulfonate (7.85 g, 46 mmol) and DMF (50 mL). The residue was purified by column chromatography (elution solvent: hexane/ethyl acetate=10/1, 4/1, 2/1) to obtain 7.12 g of the title compound as a colorless oily substance (98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536197B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-157ef90c9b174bd2b69c67455a7bca91 |
| 出典メモ | uspto-grants-2013_09 |