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HRID 1908896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/1908896
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 反応物 | (S)-Methyl 2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate | HCID 53393313 | — |
| 反応物 | (3'-(Hydroxymethyl)-6-methyl-4-[3-(methylsulfonyl)propoxy]biphenyl-2-yl)methyl acetate | HCID 59342573 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Hexane | HCID 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]acetate | HCID 59342597 | 79% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08598226B2 |
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| 出典データセット | uspto-grants-2013_12 |
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| ORD ID | ord-4972cc02cce844a282d247a4431aa63e |
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| 出典メモ | uspto-grants-2013_12 |
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