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3-Chloro-2-methyl-1-propene → tert-Butyl 4,4-dimethoxy-3-[(2-methyl-2-propen-1-yl)oxy]piperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloro-2-methyl-1-propene | HCID 11241 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate | HCID 11425480 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | tert-Butyl 4,4-dimethoxy-3-[(2-methyl-2-propen-1-yl)oxy]piperidine-1-carboxylate | HCID 86712356 | 76.9% |
反応手順
The same operation as in Example (90a) was performed using tert-butyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate (5.2 g, 20 mmol), sodium hydride (55% content, 1.31 g, 30 mmol), 3-chloro-2-methyl-1-propene (3.63 g, 40 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 4.85 g of the title compound as a colorless oily substance (77%).
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-336b16482f454c9880505ef8c50e2311 |
| 出典メモ | uspto-grants-2013_09 |