関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 7-(3-chloropropoxy)-6-methoxy-1H-quinazolin-4-one | HCID 178486769 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Chloro-7-(3-chloropropoxy)-6-methoxyquinazoline | HCID 57447227 | 78% |
反応手順
To a solution of the intermediate from Step 4 (3.00 g, 11.16 mmol) in toluene (30 mL) in a pressure vessel was added phosphorous oxychloride (8 mL). The mixture was heated to 125° C. for 5 hours. Completion of the reaction was monitored by LCMS. The mixture was concentrated to dryness and excess ethyl acetate was added. The solution was washed with water and brine and was dried (Na2SO4) and concentrated to afford the pure compound 4-chloro-7-(3-chloro-propoxy)-6-methoxy-quinazoline (2.51 g, 78%) as a yellow solid. 1H NMR (300 MHz, DMSO-d6) δ 8.85 (s, 1H), 7.48 (s, 1H), 7.35 (s, 1H), 4.35 (t, 2H), 4.00 (s, 3H), 3.75 (t, 2H), 2.25 (q, 2H). LC-MS (ESI)m/z 287 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09320739B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-bd76335f28a84b6c96c4d33b08f4f83e |
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| 出典メモ | uspto-grants-2016_04 |
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