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HRID 256836作成日:2026年10月27日

Ethyl Acetate → rac-3,4-Dihydro-2,5,7,8-tetramethyl-2-[(3-pyridinyl)ethynyl]-2H-1-benzopyran-6-ol

https://huagongshe.com/reaction/256836

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetateHCID 8857—
反応物3-BromopyridineHCID 12286—
反応物rac-3,4-dihydro-2-ethynyl-2,5,7,8-tetramethyl-2H-1-benzopyran-6olHCID 14478563—
溶媒DichloromethaneHCID 6344—
生成物rac-3,4-Dihydro-2,5,7,8-tetramethyl-2-[(3-pyridinyl)ethynyl]-2H-1-benzopyran-6-olHCID 15171813—

反応手順

Rac-3,4-dihydro-2-ethynyl-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol, 4.6 g, was reacted as described in Example 4 with 4.74 g of 3-bromopyridine. The reaction time was extended to 18 hours. The product was isolated by chromatography over 150 g of silica gel using 10% (v/v) of ethyl acetate in methylene chloride for elution. Crystallization of the combined clean fractions from ethyl acetate/hexane gave off-white crystals with m.p. 172°-175° C. The analytical sample was recrystallized from tetrahydrofuran/hexane and had m.p. 175°-178° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05260294
出典データセットuspto-grants-1993_11
ORD IDord-ef63629a95bb4a5d9d16afb8510bb459
出典メモuspto-grants-1993_11