참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phenol | HCID 996 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Chloro-5-nitrophenol | HCID 69264 | — |
| 반응물 | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| 촉매 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | 1-Chloro-2-(3-methyl-2-butenyloxy)-4-nitrobenzene | HCID 12985690 | — |
반응 단계
A reaction mixture of 2-chloro-5-nitrophenol (50.6 g), anhydrous potassium carbonate (44.5 g), tetrabutylammonium bromide (4.7 g) and 4-bromo-2-methyl-2-butene (53.3 g, 90%) in methyl ethyl ketone (263 mL) was stirred at ambient temperature overnight. TLC of the reaction mixture showed traces of phenol remaining. Additional prenyl bromide (1 mL) was then added to the reaction mixture and stirred for 2 hours. The solvent was then removed from the reaction mixture. The residue of the reaction mixture was then treated with water and extracted into diethyl ether. The extract was washed with 2N sodium hydroxide and water, dried (MgSO4), filtered, and evaporated, to leave a brown solid which was recrystallised from ethyl acetate/isopropyl alcohol to give 1-chloro-2-(3-methyl-2-butenyloxy)-4-nitrobenzene, 49.5 g, a beige solid, a single spot on TLC (ethyl acetate:hexane, 20:80).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06710077B1 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-838b54af43ff4a799efbc77e83ff702c |
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| 출처 메모 | uspto-grants-2004_03 |
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