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HRID 132674作成日:2026年10月27日
Ammonium Chloride → 8-[4-(4,4-Dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenyl]-1,4-dioxaspiro[4,5]decan-8-ol
https://huagongshe.com/reaction/132674
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-(4-Bromophenyl)-4,4-dimethyl-4,5-dihydrooxazole | HCID 403395 | — |
| 反応物 | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 8-[4-(4,4-Dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenyl]-1,4-dioxaspiro[4,5]decan-8-ol | HCID 59836702 | — |
反応手順
A solution of 8 g of 2-(4-bromophenyl)-4,4-dimethyl-4,5-dihydro-1,3-oxazole (31.5 mmol) in 15 ml of anhydrous THF is poured dropwise onto 956 mg of Mg (39.3 mmol) in such a way as to maintain the mixture at the reflux temperature and the mixture is refluxed for 2.5 hours. The mixture is cooled to room temperature and a solution of 5.41 g of 1,4-cyclohexandione monoethyleneacetal (34.65 mmol) in 20 ml of anhydrous THF is added to it dropwise. The mixture is stirred at room temperature for 1.5 hours and then at reflux temperature for 1 hour. The mixture is poured into 500 ml of a 10% NH4Cl solution and extracted with ethyl acetate. The organic phase is dried and, after filtration, the solvent is evaporated off under reduced pressure. The residue is crystallized in ethyl acetate. The product of the title is obtained in the form of a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07388031B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-e74c7a91e3f24a36955ec31da46d9a1c |
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| 出典メモ | uspto-grants-2008_06 |
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