참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phloroglucinol | HCID 359 | — |
| 반응물 | 2-Mercaptobenzoic Acid | HCID 5443 | — |
| 반응물 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 촉매 | Methanesulfonic Acid | HCID 6395 | — |
| 생성물 | 1,3-dihydroxy-9H-thioxanthen-9-one | HCID 11288016 | 69% |
반응 단계
A mixture of phosphorous pentoxide (3.71 g, 26.15 mmol) and methane sulfonic acid (27.05 mL, 0.42 mmol) was stirred at 90° C. for about one hour until a clear solution was obtained. To the reaction solution were added thiosalicylic acid (1.04 g, 6.76 mmol) and phloroglucinol (1.02 g, 8.11 mmol), followed by stirring at 70° C. for 10 minutes. After the reaction was completed, the reaction mixture was poured in 1 L of ice water. The resulting precipitate was allowed to stand at 4° C. overnight, combined, washed with water, and then dried under reduced pressure to give an orange solid compound. This compound was separated and purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:1 (v/v)) to give a yellow solid compound (1.14 g, 51.1%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846749B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-1b328ce19ee946a4a8db17dbdac99565 |
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| 출처 메모 | uspto-grants-2014_09 |
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