참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| 반응물 | 1-Oxa-6-thiaspiro(2.5)octane | HCID 18753101 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 86697202 | HCID 86697202 | — |
반응 단계
To a solution of 4-bromo-3,5-dimethylphenol (700 mg) in N,N-dimethylformamide (7 mL) is added Cs2CO3 (1.7 g) and 1-oxa-6-thiaspiro[2.5]octane (586 mg). The mixture is stirred for 12 hour at 100° C. The mixture is diluted with water and extracted twice with ethyl acetate. The combined organic phases are washed with water and brine, dried (MgSO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→60:40) to give the title compound. Yield: 986 mg; LC (method 7): tR=1.14 min; Mass spectrum (ESI+): m/z=348 [M+NH4]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08642585B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-639a96b0f51546069b1722dfdf48e51f |
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| 출처 메모 | uspto-grants-2014_02 |
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