참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Methyl 4-ethoxy-5-methoxy-2-(dimethylaminomethyleneamino)benzoate | HCID 10779127 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-Quinolinecarbonitrile, 7-ethoxy-1,4-dihydro-6-methoxy-4-oxo- | HCID 10490472 | 83.1% |
반응 단계
Added 54.0 ml (135 mmol) n-butyl lithium to 150 ml THF and chilled to -78° C. under N2. Added dropwise over 20 minutes 7.05 ml (135 mmol) acetonitrile in 200 ml THF. Stirred 15 minutes and added a solution of 17.99 g (64.2 mmol) methyl 4-ethoxy-5-methoxy-2-(dimethylaminomethyleneamino)benzoate in 150 ml THF dropwise over 20 minutes. Let stir for 0.5 hour at -78° C. Added 11.0 ml (193 mmol) acetic acid and warmed gradually to 25° C. After 2.5 hours, stripped solvent, slurried residue with water, collected solids and dried in vacuo, giving 13.025 g of yellow solid: mass spectrum (electrospray m/e): M+H=245.2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06002008 |
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| 출처 데이터셋 | uspto-grants-1999_12 |
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| ORD ID | ord-f7e54413662a4215af8b2ab042f89805 |
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| 출처 메모 | uspto-grants-1999_12 |
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