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Iodoethane → 8-Ethoxy-1,4-dioxaspiro[4.5]decane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,4-Dioxaspiro(4.5)decan-8-ol | HCID 567352 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 8-Ethoxy-1,4-dioxaspiro[4.5]decane | HCID 567358 | 55.2% |
反応手順
Sodium hydride (506 mg, 12.65 mmol) was added to a solution of 1,4-Dioxa-spiro[4.5]decan-8-ol (2 gm, 12.65 mmol) in dry THF (20 mL) at 0° C. After 15 minutes, ethyl iodide (2 gm, 12.65 mmol) was added and the mixture was allowed to stir at RT overnight. After removing the THF under reduced pressure, the mixture was poured into ice cold water and extracted into ethyl acetate. The crude product was purified by flash column chromatography (EtOAc:Hexane 5:95) to isolate the title compound (1.3 gm, 55%). 1H NMR (CDCl3, 500 MHz): δ 1.2 (t, 3H, J=7), 1.45-1.92 (m, 8H), 3.4 (m, 1H), 3.45 (m, 2H), 3.98 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08399433B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-3cd1ad02502040dea7a54b5425ebf52f |
| 出典メモ | uspto-grants-2013_03 |