関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Chromanone | HCID 68110 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4H-1-Benzopyran-4-one, 2,3-dihydro-, oxime | HCID 4486698 | — |
反応手順
A quantity (18.4 g.) of 4-chromanone was dissolved in 100 ml. ethanol with heating to the boiling temperature. To this hot solution was added 18.4 g. hydroxylamine hydrochloride and a hot aqueous solution of sodium acetate (36.8 g.) that had been dissolved in 50 ml. water heated on a steam bath. The reaction mixture was heated at the reflux temperature for 1.5 hrs. when a thin layer chromatogram indicated that the reaction was completed. After cooling the mixture to about 10° C., crystals formed. The crystals were collected on a filter, washed with water, and dried in air. There was thus obtained 18.63 g. of 4-chromanone oxime that had a melting point at 139° to 142° C. Recrystallization from methanol gave 16.5 g. of the compound having the same melting point (139° to 142° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04065574 |
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| 出典データセット | uspto-grants-1977_12 |
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| ORD ID | ord-a250119075af42cf88b2241e253ffbda |
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| 出典メモ | uspto-grants-1977_12 |
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