참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2,4-Dichlorophenethyl alcohol | HCID 2734099 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | Methyl 4-chloro-3-hydroxybenzoate | HCID 11819787 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-Chloro-3-[2-(2,4-dichloro-phenyl)-ethoxy]-benzoic Acid Methyl Ester | HCID 69652287 | — |
반응 단계
2.0 g (10.72 mmol) of 4-Chloro-3-hydroxy-benzoic acid methyl ester was dissolved in 20 ml of anhydrous tetrahydrofuran. To this solution was added 2.25 g (11.79 mmol) of 2-(2,4-Dichlorophenyl)-ethanol, 10.71 g (equivalent to 32.2 mmol PPh3) of triphenylphosphine derivatized polystyrene and 5.6 g (32.2 mmol) of DEAD. The solution was shaken for 16 h at RT. The polymer was filtered off and washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was taken-up in ethyl acetate and the solution was washed three times with water and twice with saturated aqueous sodium chloride. The organic phase was dried with magnesium sulphate, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel eluting with ethyl acetate/n-heptane (1/6).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07067665B2 |
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| 출처 데이터셋 | uspto-grants-2006_06 |
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| ORD ID | ord-c10d2f30aacc4470976dcd5c2f89ffcf |
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| 출처 메모 | uspto-grants-2006_06 |
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