참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Imidazole | HCID 795 | — |
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | Benzylamine | HCID 7504 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-Methylimidazolidine-2,4,5-trione | HCID 123196 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | HCID 178481629 | HCID 178481629 | 62% |
반응 단계
To a solution of 1-methyl-imidazolidine-2,4,5-trione (Example 1.3, Part A) (800 mg, 6.25 mmol), imidazole (467 mg, 6.87 mmol), N,N-dimethylaminopyridine (cat.) and triethylamine (1.82 mL, 13.1 mmol) in chloroform (13 mL) was added chlorotrimethylsilane (1.67 mL, 13.1 mmol) dropwise at room temperature under a nitrogen atmosphere, and the reaction mixture was stirred for 2 h. Benzylamine (0.75 mL, 6.87 mmol) was added and the reaction mixture was stirred for a further 22.5 h. The reaction mixture was diluted with chloroform and water and the chloroform extracts were dried and evaporated. The crude product was purified by column chromatography (PS with gradient elution to DCM:EtOAc 3:1) to give the product as a colourless solid (838 mg, 62%), mp 152-154° C. δH (300 MHz, CD3CN) 7.95 (v br s, 1H, NH), 7.41-7.27 (m, 5H, PhH), 4.64 (s, 2H, CH2), 2.95 (s, 3H, CH3). Mass spectrum (ESI) m/z 218 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08835629B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-acce0bf81faf4463902c8f37549108b5 |
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| 출처 메모 | uspto-grants-2014_09 |
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