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3-Bromo-1,1,1-trifluoro-2-propanone → 2-Propanone,3-bromo-1,1,1-trifluoro-, oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromo-1,1,1-trifluoro-2-propanone | HCID 79008 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Propanone,3-bromo-1,1,1-trifluoro-, oxime | HCID 2782273 | — |
反応手順
To a solution of 2.5 g of 1-bromo-3,3,3-trifluoropropan-2-one in 15 mL of chloroform (passed through a pad of basic alumina) was added a solution of hydroxylamine hydrochloride in 2.5 mL of water and the mixture heated to reflux. After 25 hours, the reaction mixture was cooled and 15 mL of H2O was added. The layers were separated and the aqueous layer was washed with 3×15 mL dichloromethane. The combined organic extracts were dried over magnesium sulfate, filtered and concentrated in vacuo. Note: As the product is a volatile liquid, excessive application of the vacuum to remove the co-solvent reduced the yield of the product. it's the product was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08053442B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-348e3198a34444be969041a504e9902d |
| 出典メモ | uspto-grants-2011_11 |