関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 反応物 | Benzenamine, 3-bromo-4-methyl- | HCID 82187 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (3-Bromo-4-methylphenyl)-(2,2-diethoxyethyl)-amine | HCID 59488813 | 80.1% |
反応手順
Under a nitrogen stream, a mixture of 3-bromo-4-methyl-phenylamine (4.94 g, 26.55 mmol), bromoacetaldehyde diethyl acetal (6.80 g, 34.50 mmol), triethylamine (5.37 mL, 38.53 mmol) and ethanol (10.3 mL) was stirred for 2 hours at 150° C. using a microwave apparatus. The resultant solution was cooled to room temperature, and then water was added thereto. The resultant mixture was extracted with dichloromethane. The organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel flash column chromatography (developing solution=ethyl acetate:n-hexane (1:10)), to thereby obtain the titled compound (6.43 g, 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08207134B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-1c17dcd5465d4098b149d97cecfc02db |
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| 出典メモ | uspto-grants-2012_06 |
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