참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4,4'-Dichlorobenzophenone | HCID 7034 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Mercaptophenol | HCID 240147 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 19387648 | HCID 19387648 | 86% |
반응 단계
A mixture of 4-mercaptophenol (50g, 0.317 mol for 80% purity), anhydrous potassium carbonate (46.9 9, g. 0.34 mol) and 150 mL of DMF was stirred and heated under nitrogen at 110°-120° C. for 90 min. The mixture was cooled to 80° C., a suspension of 4,4'-dichloro-benzophenone (40.1 g, 0.16 mol) in 100 mL DMF was added over 5 min and the mixture was stirred and heated under reflux for 4 h. After cooling to room temperature, there was added 400 mL of water and enough conc. HCl to adjust the pH to ca. 2. After stirring for 1 h, the pale yellow solid was filtered, washed with water and recrystallized from aqueous ethanol to afford 4,4'-bis(4-hydroxyphenylthio)benzo-phenone as pale yellow microcrystals, 59 g (86% yield), mp 219°-221° C. 1H NMR (DMSO-d6) was consistent with the structure with a sharp singlet for OH at δ 10.02 and four sets of doublets for the aromatic protons ranging from δ 7.61 to 6.99.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05208299 |
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| 출처 데이터셋 | uspto-grants-1993_05 |
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| ORD ID | ord-4748d0991efa4d3ab69ba93b52fc4181 |
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| 출처 메모 | uspto-grants-1993_05 |
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