참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | (2-Methoxy-5-methylphenyl)(phenyl)methanone | HCID 249273 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 촉매 | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-Methoxy-4-methyl-2-(1-phenyl-vinyl)-benzene | HCID 11356533 | 83% |
반응 단계
To a suspension of 7.58 g (21.2 mmole) methyltriphenylphosphoniumbromide in 15 ml abs. THF at room temperature within 10 minutes 17.0 ml (21.2) n-butyllithium (1.25M in n-hexane)are added dropwise. The reddish solution obtained is cooled to −78° C. and then within 15 minutes a solution of 3.70 g (16.3 mmole) 2-methoxy-5-methyl-benzophenone in 5 ml abs. THF is added. Agitation is performed initially for 20 minutes at −78° C. and for a further 8 h at room temperature. Then 80 ml water are added to the reaction mixture and extracted twice with 50 ml diethylether in each case. The purified organic phases are then dried through magnesium sulphate and the solvent is removed. Purification of the raw product obtained takes place by column chromatography on silica gel with toluene as the solvent. 3.03 g (13.5 mmole, 83%) 1-methoxy-4-methyl-2-(1-phenyl-vinyl)-benzene are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06809225B2 |
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| 출처 데이터셋 | uspto-grants-2004_10 |
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| ORD ID | ord-2928a1ae3bd549cb9f1e9c91bee88482 |
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| 출처 메모 | uspto-grants-2004_10 |
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