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HRID 631257作成日:2026年10月26日

Phosphorus oxychloride → 4-Chloro-7-(3-chloropropoxy)-6-methoxyquinazoline

https://huagongshe.com/reaction/631257

反応式

関与物質

役割名称HCID仕込み量
反応物Phosphorus oxychlorideHCID 24813—
反応物7-(3-chloropropoxy)-6-methoxy-1H-quinazolin-4-oneHCID 178486769—
溶媒TolueneHCID 1140—
生成物4-Chloro-7-(3-chloropropoxy)-6-methoxyquinazolineHCID 5744722778%

反応条件

温度125 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US09320739B2
出典データセットuspto-grants-2016_04
ORD IDord-bd76335f28a84b6c96c4d33b08f4f83e
出典メモuspto-grants-2016_04