참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 7-Methyl-2-quinolone | HCID 77673 | — |
| 반응물 | 1,3-Dioxolane, 2-(bromomethyl)- | HCID 78068 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-(1,3-Dioxolan-2-ylmethyl)-7-methylquinolin-2(1h)-one | HCID 59397835 | — |
반응 단계
To 6.3 mL of a dimethyl sulfoxide solution containing 1.1 g of 2-bromomethyl-1,3-dioxolane, 1.0 g of 7-methylquinolin-2(1H)-one and 3.1 g of cesium carbonate were added, and the mixture was stirred at 60 to 70° C. for 1 hour. The reaction mixture was added with ethyl acetate, water and an aqueous saturated sodium hydrogen carbonate solution. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with water 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 [eluent; hexane:ethyl acetate=2:3] to obtain 0.60 g of a brown oily substance, 1-(1,3-dioxolan-2-ylmethyl)-7-methylquinolin-2(1H)-one.
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-9041a22baa42428fbde1e34aa3e447f7 |
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| 출처 메모 | uspto-grants-2013_09 |
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