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HRID 591422作成日:2026年10月27日

Tributylphosphine → Methyl(4,7-dimethyl-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate

https://huagongshe.com/reaction/591422

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(6-hydroxy-4,7-dimethyl-1-benzothiophen-3-yl)acetateHCID 121004271—
溶媒TetrahydrofuranHCID 8028—
生成物Methyl(4,7-dimethyl-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetateHCID 11866700571.8%

反応手順

To a mixture of tri-n-butylphosphine (0.196 mL), (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (105 mg), methyl(6-hydroxy-4,7-dimethyl-1-benzothiophen-3-yl)acetate (130.9 mg) and THF (5.0 mL) was added ADDP (198 mg) at room temperature. The mixture was stirred at room temperature overnight under nitrogen atmosphere. The mixture was concentrated in vacuo. To the residue was added IPE, and the precipitate was filtered off. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (159 mg) as solid. The solid was crystallized from EtOAc-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-6ee8ad386e8b49789e726bac523dd442
出典メモuspto-grants-2016_01