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HRID 75040作成日:2026年10月26日

Sodium Carbonate → HCID 178427348、化合物

https://huagongshe.com/reaction/75040

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物5-fluoro-1-((4-methylphenyl)sulfonyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrrolo(2,3-b)pyridineHCID 67285690—
反応物HCID 178454306HCID 178454306—
触媒Palladium--triphenylphosphane (1/1)HCID 15220664—
溶媒1,2-DimethoxyethaneHCID 8071—
生成物HCID 178427348HCID 178427348—

反応条件

温度120 °C

反応手順

Degassed a solution of (Z)-tert-butyl (tert-butoxycarbonylamino) ((1R,3S)-3-(2-chloro-5-fluoropyrimidin-4-ylamino)cyclohexylamino) methylenecarbamate, 70b, (0.200 g, 0.411 mmol), 5-fluoro-1-(p-tolylsulfonyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrrolo[2,3-b]pyridine, 44a, (0.205 g, 0.493 mmol) and Na2CO3 (0.616 mL of 2M solution, 1.232 mmol) in dimethoxyethane (15 mL) for 30 min. To the mixture was added palladium triphenylphosphane (0.023 g, 0.021 mmol) and the reaction mixture was heated in a pressure tube at 120° C. for 45 min. The reaction mixture was filtered through a pad of celite and the filtrate concentrated in vacuo. Attempted purification of the resulting residue by silica gel chromatography (10% MeOH/CH2Cl2) yielded a mixture containing mostly desired product that was used without further purification: LCMS RT=2.30 (M+H) 641.02.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08829007B2
出典データセットuspto-grants-2014_09
ORD IDord-b8ffd87addd14b6f96c8bf97d1460c3f
出典メモuspto-grants-2014_09