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HRID 591406作成日:2026年10月25日

Tributylphosphine → Methyl(4-chloro-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate

https://huagongshe.com/reaction/591406

反応式

関与物質

役割名称HCID仕込み量
反応物TributylphosphineHCID 13831—
反応物1,1'-(Azodicarbonyl)dipiperidineHCID 73042—
反応物(2-Methyl-6-(trifluoromethyl)pyridin-3-yl)methanolHCID 2760122—
反応物Methyl(4-chloro-6-hydroxy-1-benzothiophen-3-yl)acetateHCID 20770824—
溶媒TetrahydrofuranHCID 8028—
生成物Methyl(4-chloro-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetateHCID 7172163289%

反応手順

To a mixture of methyl(4-chloro-6-hydroxy-1-benzothiophen-3-yl)acetate (110 mg) and THF (dry) (5 mL) were added (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (82 mg), tri-n-butylphosphine (0.159 mL), and ADDP (130 mg) at room temperature. The mixture was stirred at room temperature for 12 h. The insoluble material was removed by filtration, and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (164 mg). The compound was crystallized from IPE-hexane.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09238639B2
出典データセットuspto-grants-2016_01
ORD IDord-c692b59b4e41434f8b4cde10088f6389
出典メモuspto-grants-2016_01