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HRID 1916721作成日:2026年10月23日

Triethylamine → HCID 69076337、化合物

https://huagongshe.com/ja/reaction/1916721

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物2-(Di-tert-butylphosphino)biphenylHCID 2734215—
反応物3-(5-Bromopyridin-2-yl)prop-2-yn-1-olHCID 13979730—
反応物p-Chlorophenylboric acidHCID 17810664—
触媒palladium(II) acetateHCID 167845—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物HCID 69076337HCID 69076337—

反応条件

温度60 °C

反応手順

Under an N2 atmosphere 1 mL (7.22 mmol) triethylamine, 23 mg (0.1 mmol) Pd(OAc)2 and 57.5 mg (0.19 mmol) biphenyl-2-yl-di-tert-butyl-phosphane are added to a solution of 500 mg (2.36 mmol) 3-(5-bromo-pyridin-2-yl)-prop-2-yn-1-ol and 600 mg (3.72 mmol) 4-chlorophenyl-boric acid in 10 mL DMF and 2.5 mL water and the reaction mixture is stirred for 8 h at 60° C. Then 400 mg (2.48 mmol) 4-chlorophenyl-boric acid are added and the mixture is stirred for a further 19 h at 60° C. The mixture is evaporated down i. vac., the residue is combined with 10 mL water and 10 mL EtOAc, the aqueous phase is saturated with NaCl, the organic phase is separated off and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography (silica gel, cyc/EtOAc3 2:1).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08618132B2
出典データセットuspto-grants-2013_12
ORD IDord-e96886e555c64fa6a9d8e7dd566e04f0
出典メモuspto-grants-2013_12