참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,3-Dioxolane, 2-(bromomethyl)- | HCID 78068 | — |
| 반응물 | 4-Acetyl-3,4-dihydroquinoxalin-2(1H)-one | HCID 2770825 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-Acetyl-1-(1,3-dioxolan-2-ylmethyl)-2-oxo-3,4-dihydro-1h-quinoxaline | HCID 59398159 | — |
반응 단계
To 15 mL of an N,N-dimethylformamide solution containing 957 mg of 4-acetyl-3,4-dihydro-2-oxo-1H-quinoxaline, 668 mg of sodium hydride was added, and the mixture was stirred at room temperature for 1 hour. Thereto was added 2.6 mL of 2-bromomethyl-1,3-dioxolane, and the mixture was stirred at 90° C. for 6 hours. The reaction mixture was cooled to room temperature, and then ethyl acetate and 1 mol/L hydrochloric acid were added thereto. The organic layer was separated, washed sequentially with water and an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [silica gel; Silica gel 60 manufactured by Kanto Chemical Co., Inc., eluent; chloroform] to obtain 1.30 g of a brown oily substance, 4-acetyl-1-(1,3-dioxolan-2-ylmethyl)-2-oxo-3,4-dihydro-1H-quinoxaline.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08524738B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-959d4246b23d4fff8931afb03244c7ba |
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| 출처 메모 | uspto-grants-2013_09 |
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