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HRID 519807作成日:2026年10月27日

Water → HCID 178438615、化合物

https://huagongshe.com/reaction/519807

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Ethyl AcetateHCID 8857—
反応物2-Diazonio-1-ethoxyprop-1-en-1-olateHCID 53440922—
反応物HCID 178438588HCID 178438588—
触媒Rhodium acetateHCID 168478—
溶媒DichloromethaneHCID 6344—
生成物HCID 178438615HCID 17843861584%

反応手順

To a solution of 4′-{[4-(trans-4-hydroxycyclohexyl)-5-oxo-7-propyl-4,5-dihydropyrazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (0.70 g) and rhodium acetate (dimer, 0.066 g) in methylene chloride (5 mL) was added dropwise a solution of ethyl 2-diazopropanoate (1.0 g) in methylene chloride (2 mL), and the mixture was stirred for 18 hr. Ethyl acetate and water were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and then with saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was crudely purified by silica gel column chromatography. This was dissolved in tetrahydrofuran (5 mL), methylmagnesium bromide (1 M tetrahydrofuran solution, 3 mL) was added dropwise at 0° C., and the mixture was stirred for 1 hr. The mixture was diluted with ethyl acetate and then saturated aqueous ammonium chloride solution was added. The mixture was extracted with ethyl acetate, and the organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a pale-yellow amorphous solid (0.45 g, 84%).

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-d9164bc27ddf4eb0aa2ac91dff1a8865
出典メモuspto-grants-2015_08