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HRID 2076604作成日:2026年10月26日

Water → Allyl (4'-{[3-(allyloxy)-2-formyl-4-(trifluoromethyl)benzyl]oxy}-3'-fluoro-1,1'-biphenyl-4-yl)acetate

https://huagongshe.com/reaction/2076604

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Allyl bromideHCID 7841—
反応物Potassium CarbonateHCID 11430—
反応物Allyl (3'-fluoro-4'-{[2-formyl-3-hydroxy-4-(trifluoromethyl)benzyl]oxy}-1,1'-biphenyl-4-yl)acetateHCID 86617402—
溶媒DimethylformamideHCID 6228—
生成物Allyl (4'-{[3-(allyloxy)-2-formyl-4-(trifluoromethyl)benzyl]oxy}-3'-fluoro-1,1'-biphenyl-4-yl)acetateHCID 8661740324%

反応条件

温度50 °C

反応手順

Potassium carbonate (148 mg, 1.07 mmol) and allyl bromide (0.091 ml, 1.1 mmol) were successively added to a solution of allyl (3′-fluoro-4′-{[2-formyl-3-hydroxy-4-(trifluoromethyl)benzyl]oxy}-1,1′-biphenyl-4-yl)acetate (476 mg, 0.975 mmol) obtained in Example (12-4) in N,N-dimethylformamide (5 ml), and the mixture was stirred at 50° C. for 1.5 hours. After the reaction mixture was poured into water and the mixture was extracted with ethyl acetate, the organic layer was successively washed with water and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. The residue obtained by removing the solvent under reduced pressure was purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=3/1) to give allyl (4′-{[3-(allyloxy)-2-formyl-4-(trifluoromethyl)benzyl]oxy}-3′-fluoro-1,1′-biphenyl-4-yl)acetate (122 mg, yield: 24%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07923573B2
出典データセットuspto-grants-2011_04
ORD IDord-9f7463a751fd4bfdaf6dfb066f3aacce
出典メモuspto-grants-2011_04