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Butyl iodide → 6-Butoxy-2,2-dimethylchroman-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butyl iodide | HCID 10962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Hydroxy-2,2-dimethylchroman-4-one | HCID 3519859 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Butoxy-2,2-dimethylchroman-4-one | HCID 11054005 | 89.2% |
反応手順
A solution of 50 g (0.26 mol) of 2,2-dimethyl-6-hydroxychroman-4-one (Example 28a) in 500 ml of DMF was added dropwise to a suspension of 9.0 g (0.3 mol) of 80% sodium hydride in 500 ml of DMF. After stirring at RT for 90 min, 49 g (0.265 mol) of iodobutane were added and the mixture was stirred at RT for a further 90 min. The reaction mixture was then concentrated in vacuo, the residue was treated with water and the mixture was extracted several times with EA. The organic phases were washed with 5 M sodium hydroxide solution, stirred with activated carbon and magnesium sulfate, filtered and concentrated. 57.6 g of 6-butoxy-2,2-dimethylchroman-4-one were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05955607 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-0e426e1ddffc4afd8e0fc805161a3a1d |
| 出典メモ | uspto-grants-1999_09 |