참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | Diphenylphosphoryl azide | HCID 123414 | — |
| 반응물 | (2-Methylpyrimidin-5-yl)methanol | HCID 14686706 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-(Azidomethyl)-2-methylpyrimidine | HCID 54595022 | — |
반응 단계
A solution of (2-methylpyrimidin-5-yl)methanol (0.82 g, 6.6 mmol) in toluene (30 mL, 300 mmol) and methylene chloride (40 mL, 600 mmol) at 0° C. was treated with diphenylphosphonic azide (2.8 mL, 13 mmol) followed by 1,8-diazabicyclo[5.4.0]undec-7-ene (2.0 mL, 13 mmol) and stirred for 2 h at 0° C. After being further stirred at rt for 16 h, the reaction mixture was diluted with water (50 mL) and DCM (50 mL). The organic layer was separated and washed with brine, dried (Mg2SO4), filtered, and concentration. The residue was purified by column to give the product as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09133122B2 |
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| 출처 데이터셋 | uspto-grants-2015_09 |
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| ORD ID | ord-dc6dc165eeaa4449bbfc8b23cb514a24 |
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| 출처 메모 | uspto-grants-2015_09 |
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