関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl 2-(2,2-dichloro-3-oxocyclobutyl)acetate | HCID 57686758 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Methyl 2-(3-oxocyclobutyl)acetate | HCID 57686718 | 36.2% |
反応手順
To a solution of (2,2-dichloro-3-oxo-cyclobutyl)-acetic acid methyl ester (2.93 g, 13.8 mmol) in AcOH (100 ml), zinc powder (4.51 g, 69.0 mmol) is added. The mixture is stirred at 100° C. for 15 hours. The mixture is filtrated and washed with AcOH. The filtrate is concentrated under reduced pressure, and the residue is dissolved in AcOEt, and washed with saturated aqueous NaHCO3 and brine. The organic layer is dried over MgSO4, and concentrated under reduced pressure to give (3-oxo-cyclobutyl)-acetic acid methyl ester (710 mg, 36%); 1H NMR (400 MHz, chloroform-d) δ ppm 2.64-2.66 (m, 2H), 2.78-2.86 (m, 3H), 3.22-3.32 (m, 2H), 3.70 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08420641B2 |
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| 出典データセット | uspto-grants-2013_04 |
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| ORD ID | ord-e0cda268fac64acead7c07115c4799d9 |
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| 出典メモ | uspto-grants-2013_04 |
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