참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl chloroformate | HCID 6586 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Bromo-2-methylphenol | HCID 16896 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 59394985 | HCID 59394985 | 86.2% |
반응 단계
4-Bromo-2-methyl-phenol (3.63 g, 19.41 mmol) was dissolved in dichloromethane (18 mL) and triethylamine (5.41 mL, 38.80 mmol), cooled to 0° C., then treated with methyl chloroformate (2.25 mL, 29.12 mmol) and allowed to warm to room temperature over 2 h. The reaction was quenched with water and the layers separated. The aqueous layer was extracted with dichloromethane and the combined organic extracts was dried over Na2SO4, filtered, and concentrated in vacuo to yield an oil that was purified by silica gel chromatography (10% ethyl acetate/hexane) to yield 4-bromo-2-methylphenyl methyl carbonate (4.1 g, 86% yield) as a white solid. 1H NMR (400.0 MHz, DMSO-d6) δ 7.56 (d, J=2.1 Hz, 1H), 7.44 (dd, J=2.3, 8.6 Hz, 1H), 7.18 (d, J=8.6 Hz, 1H), 3.84 (s, 3H), 2.15 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08367660B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
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| ORD ID | ord-236f7d5495ee48bfae87437329164ba7 |
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| 출처 메모 | uspto-grants-2013_02 |
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