関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chloro-6,7-dimethoxyquinoline | HCID 459610 | — |
| 反応物 | 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride | HCID 66820137 | — |
| 溶媒 | 1-Methylpyrrolidine | HCID 8454 | — |
| 生成物 | 4-[6,7-Bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine | HCID 66819980 | 17% |
反応手順
A mixture of 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (300 mg, 1.13 mmol), 4-chloro-6,7-dimethoxyquinoline (253 mg, 1.13 mmol), and potassium carbonate (470 mg, 3.40 mmol) in N-methylpyrrolidine (2 mL) was stirred at 160° C. for 17 h. Ethyl acetate (75 mL) was added and the mixture was washed with water (3×25 mL) and brine (25 mL), dried over sodium sulfate, and concentrated. Column chromatography on silica (dichloromethane:methanol 95:5) afforded 4-[6,7-bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine (80 mg). MS (EI) for C20H19BrN2O3: 416 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08648066B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-0f6eff0172b3404281ea183c831fa07d |
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| 出典メモ | uspto-grants-2014_02 |
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