Potassium Acetate → 5-(2-(2-methylpyrid-3-yl)-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl)-1-(2,4-difluorophenyl)-1H-1,2,4-triazole

関与物質

役割	名称	HCID	仕込み量
反応物	Potassium Acetate	HCID 517044	—
反応物	2-Methylpyridine-3-boronic acid	HCID 20111647	—
反応物	9-Chloro-2-[2-(2,4-difluoro-phenyl)-2H-[1,2,4]triazol-3-yl]-4,5-dihydro-6-oxa-1-thia-10-aza-benzo[e]azulene	HCID 57900309	—
触媒	HCID 178418397	HCID 178418397	—
溶媒	Water	HCID 962	—
溶媒	Acetonitrile	HCID 6342	—
生成物	5-(2-(2-methylpyrid-3-yl)-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl)-1-(2,4-difluorophenyl)-1H-1,2,4-triazole	HCID 57900382	70%

反応手順

5-(2-(Chloro)-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl)-1-(2,4-difluorophenyl)-1H-1,2,4-triazole (50 mg, 0.1 mmol) was dissolved in 1 ml acetonitrile and 1 ml water, with potassium acetate (39.9 mg, 0.406 mmol). The solution was degassed by bubbling with nitrogen for 5 min. 2-Methylpyridin-3-ylboronic acid (21.4 mg, 0.156 mmol) was added, then tetrakis(triphenylphosphine)palladium(0) (19 mg, 0.016 mmol). The reaction was microwaved at 300 watts, 140° C. for 20 minutes, cooled to room temperature, and extracted with ethyl acetate. The combined organics were concentrated and purified by reverse phase HPLC to give 474 (70% yield). MS: (ESI+)=474.0

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08846762B2
出典データセット	uspto-grants-2014_09
ORD ID	ord-5360320f4bcc40679b54902500f5fbc6
出典メモ	uspto-grants-2014_09