참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | Diphenylphosphoryl azide | HCID 123414 | — |
| 반응물 | 1-(2-Methylpyrimidin-5-yl)ethanol | HCID 54772447 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-(1-Azidoethyl)-2-methylpyrimidine | HCID 58103592 | — |
반응 단계
To a stirred mixture of 1-(2-methylpyrimidin-5-yl)ethanol (2.48 g, 17 mmol) and diphenylphosphonic azide (9.3 mL, 41 mmol) in toluene (54.5 mL) at 0° C. was added neat 1,8-diazabicyclo[5.4.0]undec-7-ene (6.2 mL, 41 mmol). The reaction mixture was stirred at 0° C. for 30 minutes and then stirred at room temperature overnight. The mixture was diluted with EtOAc (100 mL) and washed with water (100 mL×2). The orangic layer was concentrated in vacuo and purified by silica gel chromatography (0-100% EtOAc/hexane) to afford a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08076345B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-643e64c4dd864f5a811b1dc935789a37 |
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| 출처 메모 | uspto-grants-2011_12 |
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