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HRID 2048631作成日:2026年10月25日

N,N-Diethylaniline → 4'-{1-[4-(1,4-Dioxaspiro[4.5]dec-8-yl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]ethyl}biphenyl-2-carbonitrile

https://huagongshe.com/reaction/2048631

反応式

関与物質

役割名称HCID仕込み量
反応物N,N-DiethylanilineHCID 7061—
反応物1,8-Diazabicyclo(5.4.0)undec-7-eneHCID 81184—
反応物Ethyl 2-[1-(2'-cyanobiphenyl-4-yl)ethyl]-3-oxohexanoateHCID 67009459—
反応物N-(1,4-dioxaspiro[4.5]dec-8-yl)-4H-1,2,4-triazol-3-amineHCID 178420920—
溶媒Hydrochloric AcidHCID 313—
生成物4'-{1-[4-(1,4-Dioxaspiro[4.5]dec-8-yl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]ethyl}biphenyl-2-carbonitrileHCID 6700969943%

反応条件

温度180 °C

反応手順

A mixture of ethyl 2-[1-(2′-cyanobiphenyl-4-yl)ethyl]-3-oxohexanoate (4.80 g), N-(1,4-dioxaspiro[4.5]dec-8-yl)-4H-1,2,4-triazol-3-amine (1.50 g), 1,8-diazabicyclo[5.4.0]undec-7-ene (0.2 mL) and N,N-diethylaniline (20 mL) was stirred at 180° C. overnight, allowed to cool and poured into 1 M hydrochloric acid (100 mL), and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography to give the title compound as a pale-yellow oil (1.50 g, 43%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08592431B2
出典データセットuspto-grants-2013_11
ORD IDord-50ba8d439ac14b37b34ec140d14b2cf2
出典メモuspto-grants-2013_11