関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2,3-Trimethoxybenzene | HCID 12462 | — |
| 反応物 | 5-Methoxy-5-oxopentanoate | HCID 6993194 | — |
| 生成物 | 5-Oxo-5-(2,3,4-trimethoxy-phenyl)-pentanoic acid methyl ester | HCID 68920007 | 77% |
反応手順
75 g of polyphosphoric acid (Acros) was charged in a 250 mL round bottom flask, followed by addition of 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methylglutarate (6.516 g, 44.60 mmol). The reaction mixture was stirred mechanically for 2.5 h at 45° C. The reaction mixture was then poured into a 1000 mL beaker containing around 250 mL of ice, and stirred well until all the product precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. No, purification required at this stage. 6.78 g (77%) of product was obtained, which was pure by NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429681B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-31bb2fbdf8ae4a799762b97d126b8f44 |
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| 出典メモ | uspto-grants-2008_09 |
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