참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-(Hexyloxy)benzoic acid | HCID 70834 | — |
| 반응물 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 반응물 | 4-(2-Aminophenethyl)-2,6-di-tert-butylphenol | HCID 19960469 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | N-[2-(3,5-di-tert-butyl-4-hydroxyphenethyl)phenyl]-N'-(4-hexyloxyphenyl)urea | HCID 19960591 | 71.1% |
반응 단계
A solution of diphenylphosphorylazide (0.93 g, 3.4 mmol), 4-hexyloxybenzoic acid (0.68 g, 3.1 mmol) and triethylamine (0.34 g, 3.4 mmol) in toluene (10 ml) was stirred at room temperature for 3.5 hrs and heated at about 90° C. for 2 hrs with stirring. After allowing the mixture to cool (under 0° C.), a solution of 4-(2-aminophenethyl)-2,6-di-tert-butylphenol (1.0 g, 3.1 mmol) in toluene (4 ml) was added dropwise. The solution was warmed up to room temperature and stirred overnight. After distilling off the solvent and purification of the residue by a silica gel column chromatography, recrystallization from ethyl acetate/hexane afforded N-[2-(3,5-di-tert-butyl-4-hydroxyphenethyl)phenyl]-N'-(4-hexyloxyphenyl)urea (1.2 g, 71% yield). m.p. 174°-176° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05621010 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-5c141c9bdd984689b832fcc33d073f7a |
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| 출처 메모 | uspto-grants-1997_04 |
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