참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Perchloric Acid | HCID 24247 | — |
| 반응물 | 5,5-Dichloro-1-morpholinopent-4-ene-1,3-dione | HCID 6605261 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2-Chloro-6-morpholinopyran-4-one | HCID 6605262 | 75.4% |
반응 단계
To a suspension of 5,5-Dichloro-1-morpholin-4-yl-pent-4-ene-1,3-dione (11.3 g, 44.9 mmol) in dioxane was added perchloric acid (11.4 ml, 0.14 mol) and the reaction was heated at 90° C. under N2 for 1 h. The reaction was cooled, neutralised with 2M NaOH (75 ml) and filtered. The aqueous layer was extracted with dichloromethane (4×30 ml) and the organic layers were combined and dried over MgSO4. The organic layer was further treated with charcoal and filtered through celite. The dark yellow filtrate was evaporated in vacuo, and the resulting solid was triturated with hexane (50 ml) and dried to give the desired compound (7.3 g, 75%) as a light yellow powder. m/z (LC-MS, ESP): 216 (M++1). 1HNMR (300 MHz, DMSO-d6): 3.3 (t, 4H), 3.65 (t, 4H), 5.4 (d, 1H), 6.25 (d, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07226918B2 |
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| 출처 데이터셋 | uspto-grants-2007_06 |
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| ORD ID | ord-1ffc3e211a8147f7af4503e11c01f4f9 |
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| 출처 메모 | uspto-grants-2007_06 |
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