참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methane | HCID 297 | — |
| 반응물 | 1,1,1-Triethoxypentane | HCID 70195 | — |
| 반응물 | Tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy)ethylcarbamate | HCID 12106200 | — |
| 반응물 | Pyridinium hydrochloride | HCID 21584435 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | tert-butyl 2-[2-(2-butyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate | HCID 21898025 | 99.9% |
반응 단계
A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (3.46 g, 10.0 mmol) in 50 mL of toluene was treated with triethylorthovalerate (2.5 mL, 14.5 mmol) and the reaction mixture was heated to reflux. A 25 mg portion of pyridinium hydrochloride was then added and refluxing was continued for 4 h. The reaction was then concentrated to dryness under reduced pressure. The residue was dissolved in 50 mL of CH2Cl2 and washed with saturated NaHCO3, H2O and brine. The organic portion was dried over Na2SO4 and concetrated to give a green oil. The green oil was dissolved in 50 mL of hot MeOH and treated with activated charcoal. The hot solution was filtered and concentrated to give 4.12 g of tert-butyl 2-[2-(2-butyl-1H-imidazo[4,5-c]quinolin-1-yl)ethoxy]ethylcarbamate as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06656938B2 |
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| 출처 데이터셋 | uspto-grants-2003_12 |
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| ORD ID | ord-a33c4bf449c64df9af0d127700e57670 |
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| 출처 메모 | uspto-grants-2003_12 |
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