참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Hexanol | HCID 12178 | — |
| 반응물 | Triphosgene | HCID 94429 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 4-[(6,7-Dimethoxyquinolin-4-yl)oxy]aniline | HCID 11594543 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 1-Ethylbutyl N-{4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}carbamate | HCID 21890820 | 90.7% |
반응 단계
4-[(6,7-Dimethoxy-4-quinolyl)oxy]aniline (100 mg) was added to toluene (10 ml) and triethylamine (1 ml), and the mixture was heated under reflux to prepare a solution. A solution of triphosgene (151 mg) in methylene chloride was then added thereto, and the mixture was heated under reflux for 10 min. Next, 3-hexanol (52 mg) was added thereto, and the mixture was further stirred with heating under reflux for 3 hr. A saturated aqueous sodium bicarbonate solution was added to stop the reaction, and the reaction solution was then extracted with chloroform, followed by washing with a 1 N aqueous hydrochloric acid solution, water, and saturated brine in that order. The extract was dried over sodium sulfate and was then concentrated. The residue was purified on a column using chloroform/methanol to give the title compound (130 mg, yield 83%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07135466B2 |
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| 출처 데이터셋 | uspto-grants-2006_11 |
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| ORD ID | ord-56e4c295f44c46558e33d7b19257bac0 |
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| 출처 메모 | uspto-grants-2006_11 |
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