참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Quinaldic Acid | HCID 7124 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Quinoline | HCID 7047 | 319.5% |
반응 단계
A 100 ml RBF equipped with magnetic stir bar and N2 inlet was charged with 356 mg (2.06 mmol, 1 eq) 2-quinaldic acid in 10 ml dry DMF. The solution was cooled to 0° C. and 415 mg (3.07 mmol, 1.5 eq) HOBt was added followed by 415 mg EDC (2.16 mmol, 1.05 eq). The reaction was stirred 2 hours at 0° C. when 1.1 g (2.06 mmol, 1 eq) of free asparagine amine in 10 ml dry DMF was added. The reaction was stirred at 0° C. for 2 hours then room temperature overnight. The reaction was poured into sat. bicarb and extracted with 2×65 mL ethyl acetate. The combined organics were washed with 5% aq. citric acid, brine, dried and concentrated to 1.4 g crude foam. Purification by flash chromatography on silica gel (100% ethyl acetate) yielded 850 mg (61%) of quinoline adduct.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05622949 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-aa6c28ca5ebe489993550699923c7862 |
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| 출처 메모 | uspto-grants-1997_04 |
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