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Hexane → 3-(3,4-Dimethyl-benzoyl)-1H-quinolin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | methyl 3-anilino-2-(3,4-dimethylbenzoyl)prop-2-enoate | HCID 178500752 | — |
| 溶媒 | Diphenyl Ether | HCID 7583 | — |
| 生成物 | 3-(3,4-Dimethyl-benzoyl)-1H-quinolin-4-one | HCID 57754515 | 80.7% |
反応手順
2-(3,4-dimethyl-benzoyl)-3-phenylamino-acrylic acid methyl ester 2a(7.00 g, 22.6 mmol) (prepared as described by Silin, O. V.; et al. Heterocycles, 2004, 63, 1883-90) was heated at 260° C. in 150 mL of diphenyl ether for 6 h, then cooled down and 100 mL of hexane was added to the reaction solution. The mixture was filtered and the solid was washed with hexane to give 5.06 g of 3-(3,4-Dimethyl-benzoyl)-1H-quinolin-4-one 3a as off-white crystals: LC-MSD, m/z for C18H15NO2 [M+H]+=278.4; HPLC retention time: 1.7 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07557213B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-1357eeddc01b472194276bf80abbd290 |
| 出典メモ | uspto-grants-2009_07 |