참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hexamethylphosphoramide | HCID 12679 | — |
| 반응물 | 1-Fluoro-4-(3-iodopropyl)benzene | HCID 18364840 | — |
| 반응물 | HCID 178463197 | HCID 178463197 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Fluoro-4-(pent-4-YN-1-YL)benzene | HCID 22279698 | 62% |
반응 단계
Subsequently, sodium acetylide (18% slurry in xylene) (50 ml) was added to hexamethylphosphoramide (20 ml) with stirring, and to the resulting mixture was furthermore added a solution of 3-(4-fluorophenyl)-1-iodopropane (7.00 g, 26.5 mmol) obtained above in dry dimethylformamide (20 ml) with stirring under ice-cooling, and then the resulting mixture was stirred at room temperature for 2 hours. After stirring, ice-cold water was added to the reaction mixture carefully with stirring under ice-cooling, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. After filtration, the solvent was removed in vacuo, and the residue was purified by flash chromatography on a silica gel column using hexane as the eluent to afford the title compound (2.67 g, yield: 62%) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08101650B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-32ac9f7b29da47319af72aa705a8a5d5 |
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| 출처 메모 | uspto-grants-2012_01 |
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