참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Acetoxybenzoyl chloride | HCID 79668 | — |
| 반응물 | 5-(Methylthio)thiazol-2-amine | HCID 351678 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(5-(Methylthio)thiazol-2-ylcarbamoyl)phenyl acetate | HCID 49775780 | 98% |
반응 단계
Under nitrogen a solution of acetylsalicyloyl chloride (1.237 g, 6.20 mmol, 1.3 eq) in THF (40 mL) was added to a stirred solution of 5-(methylthio)thiazol-2-amine? (700.0 mg, 4.79 mmol, 1.0 eq) in dry THF (mL). This was followed by the addition of triethylamine (0.67 mL, 4.79 mmol, 1.0 eq). The reaction mixture was stirred at room temperature and monitored by TLC. After two hours, reaction was filtered through sintered funnel and solvent removed in vacuo. The crude product was dissolved in EtOAc (150 mL) and washed twice each with 1M HCl and saturated aq. sodium hydrogen carbonate solutions. The organic fraction was dried over MgSO4 followed the removal of solvent. Flash column chromatography yielded the pure product 69 (1.450 g, 98%) as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08124632B2 |
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| 출처 데이터셋 | uspto-grants-2012_02 |
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| ORD ID | ord-59cc6828a1a84e3288dd8be0d09726b9 |
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| 출처 메모 | uspto-grants-2012_02 |
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