참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium ethanethioate | HCID 23670855 | — |
| 반응물 | Methyl 1-(iodomethyl)cyclohexanecarboxylate | HCID 58947958 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Acetylsulfanylmethylcyclohexanecarboxylic acid methyl ester | HCID 58947950 | 81.4% |
반응 단계
To a cold solution of crude 1261-B (109 mmol) in DMF (90 ml) was added Potassium thioacetate (1.2 equiv, 131 mmol, 15 g) maintaining temperature below 30° C. The reaction was stirred for 18 h then cooled to 10° C. and water (160 mL) was added. Reaction was extracted with EtOAc and washed with NaHCO3 sat., then brine. The dark organic layer was dried over MgSO4, filtered and concentrated down to a dark oil. Purification—HPFC (High Pressure Flash Chromatography) 75+M prepacked silica cartridge (1 to 5% EtOAc), UV collection. After concentration, 20.43 g of product 1261-C was obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07816326B2 |
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| 출처 데이터셋 | uspto-grants-2010_10 |
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| ORD ID | ord-7cd4ff6cd3d54d78a469a9eca91840b5 |
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| 출처 메모 | uspto-grants-2010_10 |
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