참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | 1,3,5-Trioxane | HCID 8081 | — |
| 반응물 | 4-Nitrobenzenesulfonamide | HCID 22784 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(3,5-Dioxapiperidin-1-yl)sulphonyl-4-nitrobenzene | HCID 22024921 | 35% |
반응 단계
4-Nitrobenzenesulphonamide (2.02 g, 10 mmol) was added to a solution of 1,3,5-trioxane (1.96 g, 20 mmol) in acetic acid (5 ml). The mixture was cooled for 5 minutes ated methanesulphonic acid (10 ml) was added slowly. The mixture was then stirred at 35° C. for 20 minutes, cooled to 0° C., diluted with water and extracted with ethyl acetate. The combined extracts were washed twice with water and twice with 5% aqueous sodium hydrogen carbonate solution, then dried and the volatiles removed by evaporation. The residue was recrystallized from ethanol to give the title compound (955 mg, 35%). NMR: 4.87 (s, 2H), 5.30 (s, 4H), 8.20 (d, 2H), 8.42 (d, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06855719B1 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-8b51693c7334427b91306a3c319f4ad9 |
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| 출처 메모 | uspto-grants-2005_02 |
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