関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 3-(Benzyloxymethyl)-2,2-dichlorocyclobutanone | HCID 10355186 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-((Benzyloxy)methyl)cyclobutanone | HCID 11819850 | — |
反応手順
Zinc dust (93.5 g, 1.44 mol) was added to a solution of 3-(benzyloxymethyl)-2,2-dichlorocyclobutanone (124 g, 0.48 mol) in glacial acetic acid (800 ml) at room temperature. The reactants were heated at 60° C. for 1 hr, after which time dry diethyl ether was added to the cooled products, which were then filtered. The residue was washed with diethyl ether and the combined filtrate and washings were concentrated under reduced pressure. The residue was dissolved in dichloromethane, which was washed with saturated NaHCO3 twice and water once. The organic phase was dried over MgSO4 and the solvent was evaporated to give an oily product, which was purified by column chromatography (Hexane: EtOAc=6:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08114994B2 |
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| 出典データセット | uspto-grants-2012_02 |
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| ORD ID | ord-5c4b9d4f19c7408b8a692fe16d039bbf |
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| 出典メモ | uspto-grants-2012_02 |
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