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HRID 519612作成日:2026年10月26日

Toluene → HCID 178440638、化合物

https://huagongshe.com/reaction/519612

反応式

関与物質

役割名称HCID仕込み量
反応物TolueneHCID 1140—
反応物Ethyl diazoacetateHCID 12192—
反応物4'-{[7-Butyl-4-(4-hydroxycyclohexyl)-5-oxo-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrileHCID 67009672—
触媒HCID 178476747HCID 178476747—
生成物HCID 178440638HCID 17844063831%

反応手順

To a mixture of 4′-{[7-butyl-4-(4-hydroxycyclohexyl)-5-oxo-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (0.61 g), rhodium(I) acetate (0.006 g) and toluene (30 mL) was added dropwise ethyl diazoacetate (0.62 mL) at 80° C., and the mixture was stirred at the same temperature for 1 hr. The reaction mixture was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography. The obtained residue was dissolved in tetrahydrofuran (15 mL), and methylmagnesium bromide (1.0 M tetrahydrofuran solution, 1.9 mL) was added at room temperature. The reaction mixture was stirred for 1 hr, 1 N hydrochloric acid was added, and the mixture was extracted with ethyl acetate. The obtained ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.22 g, 31%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09115136B2
出典データセットuspto-grants-2015_08
ORD IDord-8d453152bd55493f99b8dc8ff47113de
出典メモuspto-grants-2015_08