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HRID 1384642作成日:2026年10月25日

Potassium Carbonate → HCID 22624909、化合物

https://huagongshe.com/reaction/1384642

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物3-(2-Chloroethoxy)pyridine hydrochlorideHCID 22624985—
反応物4-(4-Chloro-2-fluorophenylamino)-7-hydroxy-6-methoxyquinazolineHCID 135513720—
溶媒WaterHCID 962—
溶媒N-methyl-2-pyrrolidoneHCID 13387—
生成物HCID 22624909HCID 2262490921.5%

反応条件

温度90 °C

反応手順

A mixture of 4-(4-chloro-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (350 mg, 1.0 mmol), (prepared as described for the starting material in Example 24), 3-(2-chloroethoxy)pyridine hydrochloride (234 mg, 1.2 mmol) and potassium carbonate (456 mg, 3.3 mmol) in NMP (20 ml) was heated at 90° C. for 2 hours. The mixture was allowed to cool, diluted with water and extracted with ethyl acetate. The combined extracts were washed with water, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with methylene chloride/methanol mixtures (100/0 increasing to 95/5) to give 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-(2-(3-pyridyloxy)ethoxy)quinazoline (95 mg, 20%). m.p. 188-190° C. 1H NMR Spectrum: (DMSOd6) 3.90(s, 3H); 4.45(m, 4H); 7.24(s, 1H); 7.18(dd, 1H); 7.2-7.60(m, 3H); 7.80(s, 1H); 8.20(d, 1H); 8.35(s, 2H); 9.50(s, 1H) MS-ESI: 441 [MH]+

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06258951B1
出典データセットuspto-grants-2001_07
ORD IDord-bc30baebc4aa45b385ddec7a86266854
出典メモuspto-grants-2001_07