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HRID 242532作成日:2026年10月24日

Ammonium fluoride → 1-[3-(7-Allyl-5,11-dihydro[1]benzoxepino[2,3-b]pyridin-5-ylidene)propyl]-4-(4-chlorophenyl)piperidin-4-ol

https://huagongshe.com/ja/reaction/242532

反応式

関与物質

役割名称HCID仕込み量
反応物Ammonium fluorideHCID 25516—
反応物AllyltributylstannaneHCID 90628—
反応物Lithium ChlorideHCID 433294—
反応物4-(4-Chlorophenyl)-1-[3-(5,11-dihydro-7-trifluoromethanesulfonyloxy[1]benzoxepino[2,3-b]pyridin-5-ylidene)propyl]piperidin-4-olHCID 73455970—
触媒HCID 178418476HCID 178418476—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
生成物1-[3-(7-Allyl-5,11-dihydro[1]benzoxepino[2,3-b]pyridin-5-ylidene)propyl]-4-(4-chlorophenyl)piperidin-4-olHCID 66757783—

反応手順

A mixture of the product of example 169 (240 mg), allyltributyltin (0.19 ml), dichlorobis(triphenylphosphine)palladium(II) (30 mg) and lithium chloride (76 mg), in dimethylformamide (3 ml) was heated under argon at 120° C. for 2 hours. Aqueous ammonium fluoride solution and ethyl acetate were added to the reaction mixture, the organic layer was separated and washed with saturated aqueous sodium chloride, and dried with magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel chromatography eluting with chloroform-methanol (10:1) to give the titled compound (180 mg).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08653096B2
出典データセットuspto-grants-2014_02
ORD IDord-cc92103c69ab464ba5bec42f7f042210
出典メモuspto-grants-2014_02