참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | tert-Butyl bromoacetate | HCID 79177 | — |
| 반응물 | 5,5-Dimethyl-3-naphthylcarbonylimidazolidine-2,4-dione | HCID 12112015 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Tert-butyl (5,5-dimethyl-3-naphthylcarbonyl-2,4-dioxoimidazolidinyl)acetate | HCID 12112014 | 70.6% |
반응 단계
5,5-Dimethyl-3-naphthylcarbonylimidazolidine-2,4-dione (686 mg) was dissolved in DMF (5 mL), and tert-butyl bromoacetate (473 mg) was added. Potassium carbonate (352 mg) was further added, and the mixture was stirred at room temperature overnight. After water was added carefully to the reaction solution, ethyl acetate (200 mL) was added, followed by extraction. The resulting organic layer was washed with 1N hydrochloric acid, an aqueous saturated sodium bicarbonate solution and a saturated brine in turn, and dried over anhydrous magnesium sulfate, and the solvent was distilled off. Further purification by silica gel chromatography (hexane:ethyl acetate=2:1) afforded white crystals. The resulting fraction was recrystallized from IPE to obtain 679 mg of white powders.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06919365B2 |
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| 출처 데이터셋 | uspto-grants-2005_07 |
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| ORD ID | ord-d77a6942f7a648a89aa1c8b0987ba8bb |
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| 출처 메모 | uspto-grants-2005_07 |
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