참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hexamethylenetetramine | HCID 4101 | — |
| 반응물 | Di-p-tolyl | HCID 11941 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 4'-Methyl-[1,1'-biphenyl]-4-carbaldehyde | HCID 1392762 | 24% |
반응 단계
Into CCl4 solvent, 2.4 g(13.3 mmol) of the compound produced in Example 1 (Compound 1) and 0.536 g(3.0 mmol) of N-bromosuccinimide were added and refluxed for 24 hours. After cooled down, the reactant was suction-filtrated and the resultant solution was washed with distilled water and then was dried with anhydrous magnesium sulfate. The dried product was dissolved again in chloroform together with 5.34 g(51.2 mmol) of hexamethylenetetraamine and refluxed for 5 hours. After the reactant was cooled down, the solvent was distilled off under reduced pressure and the residue was refluxed severely in acetic acid/H2O(17 mL/17 mL) at 120° C. for 2 hours. Finally, 7 mL of HCl was added to be refluxed. After cooled down, the reactant was extracted with methylene chloride. The solution was distilled off under reduced pressure and the residue was purified through the column chromatography (silica gel, ethyl acetate/n-hexane=1:3) to be dried. Yield; 24%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07592475B2 |
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| 출처 데이터셋 | uspto-grants-2009_09 |
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| ORD ID | ord-f94605f221fa4e2ba1a3ca2ab5b8973f |
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| 출처 메모 | uspto-grants-2009_09 |
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