참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 반응물 | Benzenamine, 3-bromo-4-methyl- | HCID 82187 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (3-Bromo-4-methylphenyl)-(2,2-diethoxyethyl)-amine | HCID 59488813 | 80.1% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08207134B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-1c17dcd5465d4098b149d97cecfc02db |
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| 출처 메모 | uspto-grants-2012_06 |
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