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Sodium hydride → 6'-bromo-4-methoxyspiro[cyclohexane-1,2'-inden]-1'(3'H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Indanone, 6-bromo- | HCID 139778 | — |
| 反応物 | 1,5-Dibromo-3-methoxypentane | HCID 58197730 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6'-bromo-4-methoxyspiro[cyclohexane-1,2'-inden]-1'(3'H)-one | HCID 58197263 | 4% |
反応手順
A mixture of 6-bromo-2,3-dihydro-1H-inden-1-one (1.037 g, 4.94 mmol) and 1,5-dibromo-3-methoxypentane (1.2 g, 4.94 mmol) in THF (16 mL) was added NaH (237.12 mg, 60%, 9.88 mmol) at room temperature. The mixture was refluxes for 3 h. The mixture was quenched with water and extracted with EtOAc. The organic layer was dried and concentrated to give the residue, which was purified by column chromatography to give 6′-bromo-4-methoxyspiro[cyclohexane-1,2′-inden]-1′(3′H)-one (60 mg, 4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889703B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-cdb90e2f3aba47afbf6ce8d36ab4449d |
| 出典メモ | uspto-grants-2014_11 |