化工社化工社 化学情報印刷レポート · 研究参考用
Chromanone → 4H-1-Benzopyran-4-one, 2,3-dihydro-, oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chromanone | HCID 68110 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4H-1-Benzopyran-4-one, 2,3-dihydro-, oxime | HCID 4486698 | — |
反応手順
To a mixture of 4-chromanone (10.00 g, 67.50 mmol) and hydroxylamine hydrochloride (7.04 g, 101 mmol) in EtOH (100 mL) was added a solution of NaOAc (16.61 g, 202.5 mmol) in H2O (30 mL). The reaction was heated to reflux for 2 h. The mixture was cooled to RT and concentrated in vacuo. The residue was diluted with H2O and acidified with 1 N HCl. The aqueous was extracted with EtOAc until tlc analysis showed no evidence of title compound in the aqueous layer. The combined organics were dried with MgSO4 and concentrated in vacuo to furnish the crude title compound which was used without further purification. MS (APCI pos) 164 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425631B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-d939d55344c149f7b163e9b26ddc39d4 |
| 出典メモ | uspto-grants-2008_09 |