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HRID 416166作成日:2026年10月24日

Tributylphosphine → methyl[(3S)-6-({2'-(acetoxymethyl)-6'-methyl-4'-[3-(methylsulfonyl)propoxy]biphenyl-3-yl}methoxy)-2,3-dihydro-1-benzofuran-3-yl]acetate

https://huagongshe.com/ja/reaction/416166

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(S)-Methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetateHCID 53393313—
反応物(3'-(Hydroxymethyl)-6-methyl-4-[3-(methylsulfonyl)propoxy]biphenyl-2-yl)methyl acetateHCID 59342573—
溶媒TolueneHCID 1140—
溶媒HexaneHCID 8058—
生成物methyl[(3S)-6-({2'-(acetoxymethyl)-6'-methyl-4'-[3-(methylsulfonyl)propoxy]biphenyl-3-yl}methoxy)-2,3-dihydro-1-benzofuran-3-yl]acetateHCID 5934259779%

反応手順

A solution of methyl[(3S)-6-hydroxy-2,3-dihydro-1-benzofuran-3-yl]acetate (0.208 g, 1.00 mmol), {3′-(hydroxymethyl)-6-methyl-4-[3-(methylsulfonyl)propoxy]biphenyl-2-yl}methyl acetate (0.360 g, 1.00 mmol) and tributylphosphine (0.324 g, 1.60 mmol) in toluene (15 mL) was stirred, 1,1′-(azodicarbonyl)dipiperidine (0.404 g, 1.60 mmol) was added, and the mixture was stirred at room temperature for 3 hr under nitrogen atmosphere. Hexane (8 mL) was added to the reaction mixture, the precipitated insoluble substance was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=30:70-70:30) to give the title compound (0.432 g, yield 79%) as a colorless oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08088821B2
出典データセットuspto-grants-2012_01
ORD IDord-c33289996cdb4626a4054fd82cb5aa9a
出典メモuspto-grants-2012_01