참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Sodium Tartrate | HCID 9357 | — |
| 반응물 | N,O-Dimethylhydroxylamine | HCID 14232 | — |
| 반응물 | Trimethylaluminum | HCID 16682925 | — |
| 반응물 | 5-(3-Fluorophenylethynyl)-nicotinic acid ethyl ester | HCID 67047762 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 86622467 | HCID 86622467 | 33.2% |
반응 단계
Sequentially add a 2 M solution of trimethylaluminum in toluene (0.64 g, 8.91 mmol) and 5-(3-fluorophenylethynyl)-nicotinic acid ethyl ester (0.24 g, 0.89 mmol), (prepared essentially as described in PREPARATION 17), to a solution of N,O-dimethylhydroxylamine (0.435 g, 4.46 mmol) in anhydrous toluene (4.0 mL) at 0° C. After 30 min, warm to room temperature and stir overnight. Dilute the reaction with ethyl acetate and an aqueous saturated solution of Rochelle salt (potassium sodium tartrate) and stir vigorously for 1 h. Separate the organic layer; dry (magnesium sulfate), filter and concentrate. Purify the resulting residue by silica gel chromatography, eluting with a linear gradient of 100:0 to 60:40 tetrahydrofuran:hexanes, to give the title compound as a pale yellow oil (0.084 g, 33%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07915424B2 |
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| 출처 데이터셋 | uspto-grants-2011_03 |
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| ORD ID | ord-587fed56830847d1b4748c7a75299f09 |
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| 출처 메모 | uspto-grants-2011_03 |
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