関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzhydrylamine | HCID 7036 | — |
| 反応物 | 3-Bromo-3-methyl-2-butanone | HCID 344911 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 3-(Benzhydrylamino)-3-methylbutan-2-one | HCID 10378301 | — |
反応手順
To the above-obtained 3-bromo-3-methylbutan-2-one (5.88 g) in methanol (30 mL), benzhydrylamine (5.0 mL) and triethylamine (7.5 mL) were added. The resultant mixture was stirred at 70° C. for 24 hours, and then cooled in air. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was sequentially washed with saturated aqueous sodium hydrogencarbonate and saturated brine, and then dried over magnesium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure, and to the solid, diethyl ether was added, and then insoluble matter was removed by filtration. The mother liquid was brought to the dryness under reduced pressure. The residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give 3-(benzhydrylamino)-3-methylbutan-2-one as an oily product (3.3 g, 34%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07622471B2 |
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| 出典データセット | uspto-grants-2009_11 |
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| ORD ID | ord-1ba1062def9a4ca19e6b16ec356f0ab2 |
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| 出典メモ | uspto-grants-2009_11 |
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