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HRID 15652作成日:2026年10月25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/reaction/15652

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US07732626B2
出典データセットuspto-grants-2010_06
ORD IDord-6a7924da036c476781bb9ebc7bbc46e5
出典メモuspto-grants-2010_06