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HRID 381267作成日:2026年10月27日

Water → 2-[3-(2-Chlorophenyl)-6-fluoro-4-oxo-3,4-dihydroquinazolin-2-yl-vinyl)pyridine-2-carbaldehyde

https://huagongshe.com/reaction/381267

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物1,4-DioxaneHCID 31275—
反応物4(3H)-Quinazolinone, 3-(2-chlorophenyl)-6-fluoro-2-methyl-HCID 64065—
反応物2,6-DiformylpyridineHCID 79485—
触媒ZincchlorideHCID 3007855—
溶媒Acetic AnhydrideHCID 7918—
生成物2-[3-(2-Chlorophenyl)-6-fluoro-4-oxo-3,4-dihydroquinazolin-2-yl-vinyl)pyridine-2-carbaldehydeHCID 86583867—

反応手順

A catalytic amount (about 100 mg) of anhydrous zinc chloride was added to a solution of 576 mg (2.0 mmol) of 3-(2-chlorophenyl)-6-fluoro-2-methyl-4(3H)-quinazolinone and 270 mg (2.0 mmol) of 2,6-pyridinedicarboxaldehyde in 20-25 mL of dioxane and 1.0 mL of acetic anhydride. The reaction mixture was heated at reflux under a nitrogen atmosphere for 3 hours until TLC indicated that the starting materials had been consumed. The cooled reaction mixture was poured into water and the mixture was extracted with ethyl acetate. The combined extracts were dried with brine and magnesium sulfate, treated with decolonizing carbon and filtered and the solvent was removed to give the desired product. This was taken up in 2:1 ether/pentane and the crystals were filtered to give 266 mg of the product, 33%, m.p. 247-248° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06306864B1
出典データセットuspto-grants-2001_10
ORD IDord-94cc04b662cc4a358cdbe22d7fa356db
出典メモuspto-grants-2001_10