참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydroquinone | HCID 785 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 4-(4-Acryloxybutoxy)benzoic acid | HCID 11032735 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 4-[4'-(4-Acryloxybutoxy)benzoyloxy]phenol | HCID 15218597 | 66.5% |
반응 단계
Oxalyl chloride (10 ml) is added at 0° C. to (2) (5 g; 19 mmol), and the mixture is stirred until the evolution of gas subsides (20 min). The excess oxalyl chloride is removed by distillation in a water-pump vacuum, the acid chloride is taken up in toluene (10 ml), the toluene solution is added at 0° C. to a solution of hydroquinone (10.5 g; 95 mmol) in pyridine (10 ml) and toluene (5 ml), and the mixture is subsequently stirred at room temperature for 24 hours. The reaction mixture is then transferred into water (200 ml), and the mixture is extracted twice with dichloromethane (50 ml each time). The organic extracts are dried using calcium chloride, hydroquinone (50 mg) is added to the filtrate, and the mixture is evaporated in a water-pump vacuum. The residue is chromatographed on silica gel (toluene/ethyl acetate (5:1), giving 4.5 g (66%) of (3).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05833880 |
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| 출처 데이터셋 | uspto-grants-1998_11 |
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| ORD ID | ord-6dc6e02f02fd4794b8c41de2bf8f3b89 |
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| 출처 메모 | uspto-grants-1998_11 |
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